СПОСОБ ЗАТВЕРДЕВАНИЯ С ПРИМЕНЕНИЕМ АНТИРАСТВОРИТЕЛЯ

FIELD: chemistry. SUBSTANCE: according to novel method liquid medium, containing at least one dissolved organic or inorganic compound, which is subject to solidification, is forced through membrane into one or several anti-solvents, or one or few anti-solvents are forced through membrane into liquid medium, which contains at least one organic or inorganic compound. Membrane is located in membrane module, has pores with size to 3mcm, membrane form is selected from pipe, fibre or spiral winding. Method is realised as continuous process. Method ensures obtaining solid particles, which include organic or inorganic compound, which are non - agglomerated. Method can be used for large volumes and allows controlling particle size. EFFECT: obtaining possibility of application for large volumes and ensuring control of particle size. 15 cl, 2 dwg, 2 tbl, 5 ex ÐÎÑÑÈÉÑÊÀß ÔÅÄÅÐÀÖÈß RU (19) (11) 2 339 364 (13) C2 (51) ÌÏÊ A61K A61K B01D B01J 9/14 (2006.01) 9/16 (2006.01) 9/02 (2006.01) 2/06 (2006.01) ÔÅÄÅÐÀËÜÍÀß ÑËÓÆÁÀ ÏÎ ÈÍÒÅËËÅÊÒÓÀËÜÍÎÉ ÑÎÁÑÒÂÅÍÍÎÑÒÈ, ÏÀÒÅÍÒÀÌ È ÒÎÂÀÐÍÛÌ ÇÍÀÊÀÌ (12) ÎÏÈÑÀÍÈÅ ÈÇÎÁÐÅÒÅÍÈß Ê ÏÀÒÅÍÒÓ (21), (22) Çà âêà: 2005136983/15, 28.04.2004 (24) Äàòà íà÷àëà îòñ÷åòà ñðîêà äåéñòâè ïàòåíòà: 28.04.2004 (30) Êîíâåíöèîííûé ïðèîðèòåò: 29.04.2003 US 60/466,761 (43) Äàòà ïóáëèêàöèè çà âêè: 20.03.2006 (73) Ïàòåíòîîáëàäàòåëü(è): Í.Â.ÎÐÃÀÍÎÍ, NL (NL) (45) Îïóáëèêîâàíî: 27.11.2008 Áþë. ¹ 33 2 3 3 9 3 6 4 (56) Ñïèñîê äîêóìåíòîâ, öèòèðîâàííûõ â îò÷åòå î ïîèñêå: US 6221398 Â1, 24.04.2001. WO 03/032951 À1, 24.04.2003. RU 2026670 Ñ1, 20.01.1995. RU 2136665 Ñ1, 10.09.1999. (85) Äàòà ïåðåâîäà çà âêè PCT íà íàöèîíàëüíóþ ôàçó: 29.11.2005 2 3 3 9 3 6 4 R U (87) Ïóáëèêàöè PCT: WO 2004/096405 (11.11.2004) C 2 C 2 (86) Çà âêà PCT: EP 2004/004506 (28.04.2004) Àäðåñ äë ïåðåïèñêè: 129090, Ìîñêâà, óë. Á.Ñïàññêà , 25, ñòð.3, ÎÎÎ "Þðèäè÷åñêà ôèðìà Ãîðîäèññêèé è Ïàðòíåðû", ïàò.ïîâ. Å.Å.Íàçèíîé, ðåã. ¹ 517 (54) ÑÏÎÑÎÁ ÇÀÒÂÅÐÄÅÂÀÍÈß Ñ ÏÐÈÌÅÍÅÍÈÅÌ ÀÍÒÈÐÀÑÒÂÎÐÈÒÅËß (57) Ðåôåðàò: Ñîãëàñíî íîâîìó ...

Verfahren zur Herstellung kristalliner Wirkstoffpartikel

Es wird ein Verfahren zur Herstellung kristalliner Wirkstoffpartikel bereitgestellt, bei dem Wirkstoff aus einer übersättigten Lösung an der Oberfläche von Partikeln des Wirkstoffs kristallisiert, wobei in einem ersten Modul eine Suspension von Wirkstoffpartikeln in einer übersättigten Lösung des Wirkstoffs einem Naßmahlen unterworfen wird, zumindest ein Teil der Suspension von Wirkstoffpartikeln in einem zweiten Modul gekühlt und gleichzeitig mit Ultraschall beaufschlagt wird, das zweite Modul mit Wirkstoffpartikelsuspension aus dem ersten Modul gespeist und die Wirkstoffpartikelsuspension nach dem Kühlen und Beaufschlagen mit Ultraschall in das erste Modul zurückgeführt wird, wobei der Suspension Wirkstofflösung und gegebenenfalls Antilösungsmittel zugeführt und Wirkstoffpartikel sowie flüssige Phase entnommen werden, wobei die relative Übersättigung des Wirkstoffs in der flüssigen Phase der Suspension, bezogen auf die gesamte flüssige Phase 90% ist und die entnommenen Wirkstoffpartikel ...

Process for making crystals

Novel apparatus and process

Eutectic extraction of solids

Purified lithium bis(fluorosulfonyl)imide (lifsi) products, methods of purifying crude lifsi, and uses of purified lifsi products

Carboxylic acid salt removal during hydrate inhibitor recovery

Carboxylic acid salt removal during hydrate inhibitor recovery

Carboxylic acid salt removal during hydrate inhibitor recovery

PROCEDURE FOR THE CRYSTALLIZATION USING HYDRODYNAMIC CAVITATION

�BERKRITISCHE ATOMISING AND BLISTERS TROCHNEN FLUIDGEST�TZTE

Rotor-stator apparatus and process for the formation of particles

Method for continuous preparation of high bulk density methionine crystal

The present invention relates to a method for the continuous preparation of high bulk density methionine crystals. The process of the method is as follows: a hydrolysate, which is obtained from a reaction of 5-(β-methylthioethyl)hydantoin and a potassium carbonate solution, is mixed with an external circulation material from a DTB neutralization crystallizer having a gas phase neutralization section; after the mixture is cooled, the mixture enters a liquid distributor of a neutralization region in the upper part of the crystallizer; the mixture is sprayed in liquid droplets or trickles into carbon dioxide gas for neutralization reaction, and then naturally falls into a crystallization region in the lower part to be mixed with a material in the region; the mixture grows on small crystals in a system to form crystals having larger particle diameters, and meanwhile new crystal nucleuses are formed; in a settling region in the middle part of the crystallization region, the crystals having larger ...

Carboxylic acid salt removal during hydrate inhibitor recovery

A method and system for precipitation and separation of carboxylic acid salts from a hydrate inhibitor solution is disclosed. The method comprises lowering the solubility of the carboxylic acid salts to force precipitation of carboxylic acid salts and separation of the precipitated carboxylic acid salts from the hydrate inhibitor solution.

Plinabulin compositions

Disclosed herein are plinabulin polymorphs, compositions, their use and preparation as therapeutic agents. In particular, some embodiments relate to plinabulin monohydrate in a crystalline form.

Pressure driven flow crystallizer

The present invention generally relates to systems and methods for pressure driven flow crystallization. In some embodiments, the system comprises a comprising a cavity and a mixing mechanism. In some embodiments, one or more inlets facilitate the transfer of one or more reagent streams to the cavity. In some such embodiments, the mixing mechanism mixes the first and second reagent streams such that a continuous crystallization and/or generation of a product (e.g., solid particles) in the fluid.

PROCESS FOR MAKING CRYSTALS

A process for preparing crystalline particles of an active principal in t he presence of ultrasonic irradiation that comprises contacting a solution o f a solute in a solvent in a first flowing stream with an anti-solvent in a second flowing stream causing the mixing thereof, wherein the flow rate rati o of the anti- solvent: solvent is higher than 20:1, and collecting crystals that are generated.

METHODS FOR EXTRACTION, PROCESSING, AND PURIFICATION OF A SELECTED FAMILY OF TARGET COMPOUNDS FROM CANNABIS

Disclosed are methods for separating, recovering, and purifying tetrahydrocannabinolic acid (THCA) salts from an organic solvent solution comprising a mixture of cannabinoids. The methods comprise solubilizing the mixture of cannabinoids in a selected C5-C7 hydrocarbon solvent, adding thereto a selected amine to thereby precipitate a THCA-amine salt therefrom, dissolving the recovered THCA-amine salt in a selected solvent and then adding thereto a selected antisolvent to thereby recrystallize a purified THCA-amine salt therefrom. The recrystallized THCA-amine salt may be decarboxylated to form a mixture of A9-tetrahydrocannabinol (A9-THC) and amine. The A9-THC amine mixture may be acidified to separate the amine from A9-THC. The recovered A9-THC may be concentrated to produce a highly purified A9-THC. Also disclosed are THCA-amine salts produced with amines selected from groups of diamines, amino alcohols, and tertiary amines.

METHOD FOR PRODUCING BIS(FLUOROSULFONYL)AMIDE ALKALI METAL SALT POWDER

The present invention addresses the problem of providing a method for producing a high-purity bis(fluorosulfonyl)amide alkali metal salt powder, wherein the reduction of the yield due to pyrolysis etc., is inhibited. The method for producing a bis(fluorosulfonyl)amide alkali metal salt powder according to the present invention comprises distilling, by using a thin-film evaporator, a solution obtained by dissolving a bis(fluorosulfonyl)amide alkali metal salt in a good solvent for the bis(fluorosulfonyl)amide alkali metal salt, such as an ester-based solvent or a nitrile-based solvent, while adding a poor solvent for the bis(fluorosulfonyl)amide alkali metal salt, such as an aromatic hydrocarbon-based solvent or a straight-chain or branched aliphatic carbon hydrogen solvent to the solution, and thereby causing the bis(fluorosulfonyl)amide alkali metal salt to be deposited.

CRYSTALLIZATION SYSTEM UTILIZING ATOMIZATION

Crystallization of an organic pharmaceutical compound is achieved by atomization of one solution and introduction of the atomized solution into a vessel containing a second solution where the solutions are mixed to form a product. The process can be performed on non-reactive constituents such as a solution containing the compound to be crystallized dissolved in a solvent and an anti-solvent solution. Alternatively, the process can be performed on reactive constituents, such as solutions of solvents containing different reactive intermediates, under proper reactive conditions. The process may be practiced continuously or in batch mode. Atomizers of the non-pressure-driven ultrasonic type or of the ultrasonic or non-ultrasonic pressure-driven type can be utilized.

METHOD FOR EXTRACTING A MACROLIDE FROM BIOMATTER

Provided is a method for obtaining a macrolide, especially tacrolimus, from biomatter.

DIVALENT ION REMOVAL FROM MONOETHYLENE GLYCOL-WATER STREAMS

A system and process for the removal of divalent ions from a MEG-water stream (10) are presented. The system includes a chemical treatment tank (5) that receives the MEG-water stream (10), means for precipitating the calcium, magnesium, and hydroxide ions that are contained in the MEG-water stream (10), means for discharging the MEG-water stream (10) from the chemical treatment tank (5), and means for recycling the discharged MEG-water stream (10) back to the chemical treatment tank (5) or routing it to a solids removal system (75). The means for precipitating the calcium, magnesium, and sulfate ions may be employed simultaneously or sequentially.

A METHOD FOR DETERMINATION OF SIROLIMUS STABILITY AND PROCESS FOR PREPARING ITS STABLE FORM

The present disclosure provides solution to the problems involved in determining the crystallinity of sirolimus. More particularly, the instant disclosure is successful in providing a method to determine crystallinity of sirolimus or its analogues using Near-Infrared [NIR] spectroscopy. Also, the instant disclosure provides a method for crystallization of sirolimus or its analogues.

POLYMORPHOUS FORM OF PITAVASTATIN CALCIUM

DEVICE AND METHOD FOR MANUFACTURING DISPERSIONS AND SOLID PHASES

Continuous production method and continuous production device for synthesizing biruea

POWERED HAND TOOL

La présente invention concerne un dispositif microfluidique comprenant au moins une chambre de cristallisation susceptible de comprendre une solution dans laquelle au moins un composé est présent selon un gradient de concentration et dans lequel la géométrie de ladite chambre de cristallisation permet de limiter les phénomènes de convection. Elle concerne également l'utilisation dudit dispositif notamment pour la cristallisation par contre-diffusion et un procédé de cristallisation.

COMPOSITION BASED ON LITHIUM BIS(FLUOROSULFONYL)IMIDE SALT

DOTA 합성

... 본 발명은 생체내 치료 및 진단 용도에 유용한 화합물의 제조 방법을 제공한다. 구체적으로, 본 발명은 1,4,7,10-테트라아자시클로도데칸-1,4,7,10-테트라아세트산 (DOTA)의 합성 방법 및 또한 DOTA 금속 킬레이트의 제조 방법을 제공한다.

PROCESSES INVOLVING THE USE OF ANTISOLVENT CRYSTALLISATION

The present invention pertains to a process to make salt compositions comprising the steps of - feeding water to a salt source to form an aqueous solution comprising said salt, - feeding said aqueous solution to a crystalliser/settler, - contacting said aqueous solution with one or more antisolvents which force the salt to crystallise, with said antisolvents exhibiting crystal growth inhibiting properties and/or crystallisation and scale inhibiting properties, and/or where one or more crystal growth inhibitors are present either in the antisolvents or the aqueous solution and/or one or more scaling inhibitors are present either in the antisolvents or the aqueous solution, - feeding an overflow of the crystalliser/settler comprising one or more antisolvents and an aqueous salt solution to a nanofiltration unit comprising a membrane to separate the one or more antisolvents from the aqueous salt solution, - removing the crystallised salt in an aqueous slurry, - optionally, recycling the one ...

Processes for producing organophosphorous compounds

The present invention relates to processes for producing organophosporous compositions having low acid content as well as processes for reprocessing partially degraded organophosporous compositions that contain high levels of phosphorous acid. In one embodiment, a process comprises: (a) receiving a solid organophosphite compound that has been recrystallized or triturated, wherein the solid organophosphite compound comprises phosphorous acid; (b) dissolving the solid organophosphite compound in a an aromatic hydrocarbon solvent in the absence of water and free amine, wherein the hydrocarbon solvent comprises an aromatic hydrocarbon, a saturated aliphatic hydrocarbon, or a mixture thereof; and (c) removing undissolved phosphorous acid from the solution, wherein the acid content of the organophosphite following step (c) is 30 ppm or less.

REVERSIBLE CONTROL OF SOLUTION SOLUBILITY USING FUNCTIONALIZED NANOPARTICLES

Aspects of the disclosure relate to methods and compositions of altering a solution through the use of readily retrievable agents (e.g., a nanoparticle) having one or more functional groups configured to undergo a solvation interaction with a component of the solution. Compositions, systems, and methods for crystallizing organic and inorganic compounds from solutions using nanoparticles surface coated with functional groups that create a supersaturated state in the solution and reversal thereof. Compositions, systems, and methods for purifying water or active pharmaceutical ingredients. Compositions, systems, and methods for increasing the solubility of a solution and reversal of the same. Compositions, systems, and methods for decreasing the solubility of a crystallized compound and reversal of the same. 1. A method of altering a solution , the method comprising combining a solution with a readily retrievable agent having one or more functional groups configured to undergo a solvation interaction with a component of the solution.2. The method of claim 1 , wherein the solvation interaction is solvation of the one or more functional groups by the solvent.3. The method of claim 1 , wherein the solvation interaction is solvation of a solute of the solution by the one or more functional groups.4. The method of claim 1 , wherein the readily retrievable agent is a nanoparticle.5. The method of claim 4 , wherein the nanoparticle is magnetic.6. The method of any preceding claim claim 4 , wherein the readily retrievable agent is surface coated with the one or more functional groups.7. The method of any preceding claim claim 4 , wherein the readily retrievable agent further comprises one or more affinity tags.8. The method of any preceding claim claim 4 , wherein the affinity tag comprises a streptavidin or biotin moiety.9. The method of any preceding claim claim 4 , further comprising:i) maintaining the combination for a period of time; andii) following step i), retrieving ...

Синтез DOTA

Изобретение относится к способу синтеза 1,4,7,10-тетраазациклододекан-1,4,7,10-тетрауксусной кислоты (DOTA), включающему (a) взаимодействие 1,4,7,10-тетраазациклододекана (циклена) с галогенуксусной кислотой и избытком основания; (b) кристаллизацию реакционной смеси, полученной на стадии (а), путем добавления в нее органического растворителя, где указанную кристаллизацию проводят при рН более 3 и менее 3,5; (c) фильтрацию водного раствора кристаллизованного на стадии (b) продукта путем нанофильтрации; (d) кристаллизацию отфильтрованного раствора, полученного на стадии (с), путем добавления в него органического растворителя. Изобретение также относится к способу получения хелатного комплекса металл-DOTA и к способу получения гадотерата меглумина. Технический результат: предложен способ синтеза 1,4,7,10-тетраазациклододекан-1,4,7,10-тетрауксусной кислоты, применимый при промышленном производстве, при котором происходит улучшенное удаление органических и неорганических примесей из неочищенной ...

СПОСОБЫ ПОЛУЧЕНИЯ ФОСФОРОРГАНИЧЕСКИХ СОЕДИНЕНИЙ

ОЧИСТКА ЗАГРЯЗНЁННОГО ВНЕСЕНИЕМ ОКСИДОВ СЕРЫ РАСТВОРИТЕЛЯ НА ОСНОВЕ АМИНА

... 1. Способ очистки загрязненного внесением оксидов серы растворителя (1) на основе амина, в котором- в загрязненный растворитель (1) вводят соединение калия и охлаждают загрязненный растворитель (1) до температуры Т, в результате чего снижается растворимость сульфата калия по сравнению с его имеющейся концентрацией,- отфильтровывают сульфат калия и получают очищенный растворитель (3),отличающийся тем, что в загрязненный растворитель (1) вводят окислитель (2), в результате чего сульфит окисляется в сульфат.2. Способ по п.1, в котором окислитель (2) и соединение калия смешивают между собой перед введением в раствор соли аминокислоты.3. Способ по п.1 или 2, в котором в качестве окислителя (2) применяют перекись водорода или озон.4. Способ по п.1 или 2, в котором количество подведенного соединения калия эквимолярно количеству кристаллизованного сульфата калия.5. Способ по п.1, в котором температура Т загрязненного растворителя (1) после охлаждения составляет от 5 до 45°C.6. Способ по п.1, в ...

ROV Cable insulation system

A ROV cable insulation system comprises insulated electric conductors 21, sheathed drain wires 22, screen tape 23, and outer protection 24, 25. The screen tape comprises a polymeric, preferably Nylon, semi-conductive tape.

Crystallisation methods

Improved loop reactor

A loop reactor comprising a head tank 1, a heat exchange column, 5 and conduits 3 and 4. The heat exchange column is provided with a tangential stirrer 6 and a means is provided for pumping fluid through the head tank, conduits and heat exchange column in a recycling loop. Preferably the flow through the heat transfer column is orderly flow. Preferably the head tank is provided with a pitched blade stirrer 2 in order to drive flow through the loop. Also disclosed is a process for crystallisation via pumping a fluid around a loop reactor comprising a head tank 1, heat exchange column 5, and conduits 3 and 4. The heat exchange column is provided with a tangential stirrer 6 and a means is provided for pumping fluid through the head tank, conduits and heat exchange column in a recycling loop.

PROCEDURE AND REACTOR FOR THE PRODUCTION OF POWDERS FOR INHALATIONAL MEDICINES

DEVICE AND PROCEDURE FOR MANUFACTURING CRYSTALLINE PARTICLES

Crystallization method and apparatus using an impinging plate assembly

Antisolvent solidification process

Carboxylic acid salt removal during hydrate inhibitor recovery

A method and system for precipitation and separation of carboxylic acid salts from a hydrate inhibitor solution is disclosed. The method comprises lowering the solubility of the carboxylic acid salts to force precipitation of carboxylic acid salts and separation of the precipitated carboxylic acid salts from the hydrate inhibitor solution.

Carboxylic acid salt removal during hydrate inhibitor recovery

A method and system for precipitation and separation of carboxylic acid salts from a hydrate inhibitor solution is disclosed. The method comprises lowering the solubility of the carboxylic acid salts to force precipitation of carboxylic acid salts and separation of the precipitated carboxylic acid salts from the hydrate inhibitor solution.

Process for rapid identification and preparation of crystalline forms

Disclosed is a method of rapid identification and preparation of a crystalline form of an organic compound by using sub-gram level of said organic compound, comprising the steps of temperature-cycled slurrying, cooling, antisolvent addition and solvent evaporation as the major crystallization steps.

PROCESSING POST-INDUSTRIAL AND POST-CONSUMER WASTE STREAMS AND PREPARATION OF POST-INDUSTRIAL AND POST-CONSUMER PRODUCTS THEREFROM

A system for and method of, processing post-consumer and post-industrial waste streams, producing active ingredients for waste stream processing, processing aqueous waste streams, preparing and collecting a multi-purpose chemical precursor, removing phosphates, nitrates, heavy metals, and other contaminants from aqueous waste streams, collecting and processing a post-consumer and post-industrial product from aqueous waste streams, administering and positioning assets and processes associated with waste stream processing, and scheduling operations for sub-systems of the system.

SYSTEMS, APPARATUS AND METHODS FOR SEPARATING ACTINIUM, RADIUM, AND THORIUM

A method of separating actinium and/or radium from proton-irradiated thorium metal. The thorium metal is irradiated to produce isotopes including thorium, actinium and/or radium. The resultant product is dissolved in solution and a selective precipitant is used to precipitate a bulk portion of the thorium. The precipitated thorium can be recovered. Chromatography is carried out on the remaining solution to remove residual thorium and to separate the actinium from the radium.

METHODS FOR EXTRACTION, PROCESSING, AND PURIFICATION OF A SELECTED FAMILY OF TARGET COMPOUNDS FROM CANNABIS

Disclosed are methods for separating, recovering, and purifying cannabidiolic acid (CBDA) salts from an organic solvent solution comprising a mixture of cannabinoids. The methods comprise solubilizing the mixture of cannabinoids in C5-C7 hydrocarbon solvents, adding thereto a selected amine to thereby precipitate a CBDA-amine salt therefrom, dissolving the recovered CBDA-amine salt in a selected solvent and then adding thereto a selected antisolvent to thereby recrystallizing a purified CBDA-amine salt therefrom. The recrystallized CBDA-amine salt may be decarboxylated to form a mixture of cannabidiol (CBD) and amine. The CBD amine mixture may be acidified to separate the amine from CBD. The recovered CBD may be concentrated to produce a highly purified CBD. Also disclosed are CBDA-amine salts produced with certain amines selected from groups of secondary amines, tertiary amines, diamines, amino alcohols, amino ethers, and highly basic amines.

PARTICLE FORMATION METHODS AND THEIR PRODUCTS

Preparation of particles of an active substance having a layer ofan additive at the particle surfaces, by dissolving both the active substance and the additive in a vehicle to form a target solution, and contacting the target solution with an anti-solvent fluid using a SEDSTM particle formation process, to cause the active substance and additive to coprecipitate. The additive is typically a protective additive, in particular a taste and/or odour masking agent. Also provided is a particulate coformulation made by the method, which has a finite gradient in the relative additive concentration, which concentration increases radially outwards from the active rich core to the additive-rich surface of the particles.

MICROFLUIDIC DEVICE FOR CRYSTALLIZATION AND CHRYSTALLOGRAPHIC ANALYSIS OF MOLECULES

La présente invention concerne un dispositif microfluidique comprenant au moins une chambre de cristallisation susceptible de comprendre une solution dans laquelle au moins un composé est présent selon un gradient de concentr ation et dans lequel la géométrie de ladite chambre de cristallisation perme t de limiter les phénomènes de convection. Elle concerne également l'utilisa tion dudit dispositif notamment pour la cristallisation par contre- diffusio n et un procédé de cristallisation.

PROCESS FOR OBTAINING SOLID MICRO- OR NANO-PARTICLES

The invention provides a novel method for obtaining solid micro -or nanoparticles with a homogeneous structure. A method is provided for obtaining solid micro -or nanoparticles with a homogeneous structure having a particle size of less than µm where the processed solid compound has the natural, crystalline, amorphous, polymorphic and other features associated with the starting compound. In accordance with the invention a method which also makes it possible to obtain solid micro -or nanoparticles with a substantially spheroidal morphology is provided.

PROCESS FOR THE CRYSTALLISATION OF A WATER-SOLUBLE COMPOUND

The invention relates to a process for the crystallisation of a water-soluble compound from a solution comprising the following steps: a)providing, in a crystallisation vessel, a solution of the water-soluble compound in a mixture of water and a solvent in which the water-soluble compound has a lower solubility than in water; b)passing vapour phase of the mixture through a sorption zone containing a water vapour sorbent to selectively adsorb water from the vapour phase to obtain a vapour phase depleted in water and enriched in the solvent and water-saturated water vapour sorbent; c)enriching the mixture in the crystallisation vessel in solvent by recycling at least part of the vapour phase depleted in water and enriched in the solvent to the crystallisation vessel or withdrawing vapour phase depleted in water from the process and adding solvent from an external source to the crystallisation vessel; d)allowing solid crystals of the water-soluble compound to precipitate from the solution ...

Method for producing particles

Process and installations to obtain precipitates easy to separate from the liquid medium

PROCESS FOR MAKING CRYSTALS

NANO & MICRO-SIZED PARTICLES OF STATIN COMPOUNDS AND PROCESS FOR FORMING SAME

A process for making micro-sized or nano-sized particles of one or more statin compounds, the process comprising the step of: (a) applying a shear force to (i) a statin solution comprising one or more statin compounds, and (ii) a statin-insoluble liquid in which said statin compounds are insoluble or at least partially insoluble, said applying being undertaken under conditions to form said micro-sized or nano-sized particles of said statin compounds.

AN APPARATUS AND PROCESS FOR PRODUCING CRYSTALS

This invention provides an oscillating baffled reactor apparatus for preparing crystalline particles of at least one substance comprising: a reactor vessel; means for supplying a first flowing stream; means for oscillating fluid within the reactor vessel; a plurality of baffles; source of ultrasonic radiation; and means for collecting said particles.

METHOD FOR PRODUCING FINE ORGANIC COMPOUND PARTICLES

A method for producing fine particles of an organic compound wherein a poor solvent in which the organic compound is slightly soluble and an solution of the organic compound which is prepared by dissolving the compound in a good solvent which is compatible with the poor solvent and can easily dissolve the organic compound are continuously mixed, to form particles of the organic compound, characterized in that the above poor solvent and the above solution of the organic compound is mixed under the irradiation of the mixture with an ultrasonic wave. The method is a method for producing fine particles of an organic compound utilizing a poor solvent precipitation method in a continuous system, and allows the rapid and uniform dispersion of an organic compound solution in a large amount of a poor solvent and as a result, allows the production of fine particles of the organic compound having a volume average particle diameter of 1 μm or less with more ease.

Polymer particle, manufacturing method thereof, and separator for battery comprising the same

The present application relates to a polymer particle manufacturing method, and according to an example of the manufacturing method and a manufacturing apparatus therefor, a reduction in energy can be achieved by simplifying a manufacturing process thereof.

Process for the preparation of isocarboxazid

This invention relates to a novel chemical process for the synthesis of N′-benzyl-5-methylisoxazole-3-carbohydrazide (Isocarboxazid) which comprises reacting 5-methyl-3-isoxazole carboxylic acid ester with benzylhydrazine or a salt thereof in an aprotic organic solvent and in the presence of an organic base.

Form C of Avibactam Sodium

The present invention relates to crystalline form C of avibactam sodium and to a process for its preparation. The invention also concerns a pharmaceutical composition comprising form C and one or more antibacterial agents, wherein at least one antibacterial agent is a beta-lactam antibiotic. The pharmaceutical composition of the present invention can be used as medicament, in particular for treatment and/or prevention of bacterial infections. 1. Crystalline form C of avibactam sodium having a powder X-ray diffractogram comprising reflections at 2-Theta angles of (6.5±0.2°) , (14.4±0.2°) , (15.5±0.2°) , (18.0±0.2°) and (19.3±0.2°) , when measured at a temperature in the range of from 20 to 30° C. with Cu-Kalpharadiation having a wavelength of 0.15419 nm.2. The crystalline form C of having less than 20% by weight of any other physical form of avibactam sodium.3. The crystalline form C of comprising no reflection at 2-Theta angles of (8.5±0.2°) claim 1 , (16.4±0.2°) and/or (17.1±0.2°) claim 1 , and/or comprising no reflection at 2-Theta angles in the range of from (6.9±0.2°) to (12.6±0.2°) claim 1 , when measured at a temperature in the range of from 20 to 30° C. with Cu-Kalpharadiation having a wavelength of 0.15419 nm.4. The crystalline form C according to characterized by having{'sup': −1', '−1', '−1', '−1', '−1, '(i) a Fourier transform infrared spectrum comprising peaks at wavenumbers of (3459±2) cm, (1690±2) cm, (1287±2) cm, (1247±2) cmand (690±2) cm, when measured at a temperature in the range of from 20 to 30° C. with a diamond ATR cell, and/or'}(ii) an equilibrium relative humidity of about 55% or less, when measured at a temperature in the range of from 20 to 30° C.5. A composition comprising{'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, '(i) crystalline form C of avibactam sodium as defined in and'}{'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, '(ii) one or more additional physical form(s) of avibactam sodium which is not the crystalline form C as ...

PROCESS AND DEVICE FOR THE PRECIPITATION OF AN ORGANIC COMPOUND

PROCESS FOR MAKING STERILE ARIPIPRAZOLE OF DESIRED MEAN PARTICLE SIZE

Patent RU2017121649A3

РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2017 121 649 A (51) МПК C07C 323/58 (2006.01) C07C 319/28 (2006.01) B01D 9/02 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ЗАЯВКА НА ИЗОБРЕТЕНИЕ (21)(22) Заявка: 2017121649, 23.12.2015 Приоритет(ы): (30) Конвенционный приоритет: 12.02.2015 CN 201510078388.1 36 (86) Заявка PCT: CN 2015/098368 (23.12.2015) (87) Публикация заявки PCT: WO 2016/127707 (18.08.2016) A Адрес для переписки: 121059, Москва, а/я 107, ООО "ПАТЕНТУС", пат. пов. Михайлову А.В. R U (57) Формула изобретения 1. Способ непрерывной подготовки кристаллов метионина высокой насыпной плотности, включающий в себя следующие этапы, на которых: (1) смешивают раствор гидролизата, содержащий калий и метионин и полученный в результате реакции 5-(β-метилмеркаптоэтил)гидантоина и раствора карбоната калия с материалом внешней циркуляции из нейтрализационного кристаллизатора с циркуляционной трубкой и перегородкой (ЦТиП), имеющего секцию газофазной нейтрализации, для формирования материала смеси; вводят материал смеси в распределитель жидкости области нейтрализации в верхней части кристаллизатора после охлаждения и распыляют в виде капель или тонких струек жидкости в зону контакта газа и жидкости для проведения реакции нейтрализации газообразным диоксидом углерода с получением нейтрализационного раствора, содержащего метионин; (2) обеспечение естественного падения нейтрализационного раствора в область кристаллизации в нижней части кристаллизатора для образования кристаллов в области кристаллизации с последующим обеспечением осаждения кристаллов, имеющих частицы большего диаметра, в патрубок для отмучивания кристаллов в зоне осаждения в средней части области кристаллизации; (3) подают кристаллы метионина в патрубок для отмучивания кристаллов через Стр.: 1 A 2 0 1 7 1 2 1 6 4 9 (54) СПОСОБ НЕПРЕРЫВНОЙ ПОДГОТОВКИ КРИСТАЛЛОВ МЕТИОНИНА ВЫСОКОЙ НАСЫПНОЙ ПЛОТНОСТИ 2 0 1 7 1 2 1 6 4 9 (72) Автор(ы): ЧЕН Чжирон (CN), ВАН Чжисюан (CN), ЧЕН Кон (CN), ВАН Чженцзиан ...

Process for Making Crystals

Crystallisation of chemical molecules

A method of forming a crystal from a molecule or a salt thereof by forming a droplet from a first liquid comprising the molecule or salt dissolved in an organic medium substantially encapsulated in a second liquid which is an oil. Suitable organic media are hydrocarbons, aromatic solvents, chlorinated solvents, fluorinated solvents, ethers, ketones, sulfoxides, alcohols, diols, ureas or phosphoramides. Suitable oils are mineral oils, paraffin oils, silicon oils or perfluorinated oils. The method can be used when only very small amounts (e.g. <1 mg) of a compound are available and can be used to explore the experimental crystallisation space including screening for optimal crystallisation conditions such as for polymorphic phases, salts, solvates and co-crystals of chemical molecules and to provide single crystals for structural determination of unknown molecules by single crystal X-ray crystallography.

PRODUCTION OF SMALL CRYSTALS

PROCEDURE FOR THE PRODUCTION OF PARTICLES AND THEIR PRODUCTS

Supercritical fluid-assisted nebulization and bubble drying

Method of preparing benzy 4-amino-3-chloro-5-fluoro-6-(4-chloro-2-fluoro-3-methoxyphenyl)picolinate

A method of preparing benzyl 4-amino-3-chloro-5-fluoro-6-(4-chloro-2-fluoro-3-methoxyphenyl)picolinate (I) from benzyl 4,5-difluoro-6-(4-chloro-2-fluoro-3-methoxyphenyl)picolinate (II) is described. The method includes the use of amination and chlorination process steps to provide the compound of Formula I.

PROCESS FOR THE PREPARATION OF MICRON-SIZE CRYSTALLINE PARTICLES USING A SOLVENT, A NON-SOLVENT AND ULTRASONIC ENERGY

The invention relates to a novel procedure for the production of a high yield of small crystalline particles of a narrow size distribution.

DOTA SYNTHESIS

The present invention provides methods for the preparation of compounds useful in vivo therapeutic and diagnostic applications. In particular, the present invention provides a method for the synthesis of 1,4,7,10-tetraazacyclododecane-1,4, 7,10- tetraacetic acid (DOTA) and also methods for the preparation of metal chelates of DOTA.

EQUIPMENT ASSEMBLY AND METHOD OF PROCESSING PARTICLES

An equipment assembly for preparing, harvesting and collecting particles is disclosed. The assembly comprises a tandem filter system with one or more high pressure filters, one or more low pressure filters and one or more collection vessel. Particles can be prepared, harvested and collected continuously, semi-continuously or in a batch-type operation. A tandem filter system and its method of use are also disclosed. Particles made with the assembly and according the instant methods are also disclosed. The assembly provides improved particle harvesting and collection over other systems and permits continuous particle formation, in particular by dispersion of a solute-containing process fluid within a supercritical anti-solvent.

METHOD FOR CRYSTALLIZATION OF A WEAKLY ACIDIC AND/OR WEAKLY BASIC COMPOUND

A method for crystallization of a weakly acidic and/or weakly basic compound having an uncharged form and at least one charged form comprises the steps of: a) providing a solution of said compound in a solvent having an initial pH- value and an initial total concentration of said compound, said initial pH- value being chosen such that the compound is present in said solution pre- dominantly in said charged form, said initial total concentration being cho- sen larger than the intrinsic solubility of said uncharged form; b) gradually changing the pH-value of said solution in a direction that leads to a decrease of said compound's solubility until reaching a predetermined target pH-value at which said solution is in a substantially saturated state and the concentration of said uncharged form is substantially equal to said intrinsic solubility thereof; and c) maintaining said solution in a substantially saturated state while allowing formation of crystals of said compound.

MICROFLUIDIC DEVICE FOR CRYSTALLIZATION AND CHRYSTALLOGRAPHIC ANALYSIS OF MOLECULES

The present invention relates to a microfluidic device comprising at least one crystallization chamber adapted for comprising a solution in which at least one compound is present according to a concentration gradient and in which the geometry of said crystallization chamber allows for the convection phenomena to be limited. The invention also relates to the use of said device, in particular for the crystallization by counter diffusion and to a crystallization method.

DESALINATION OF AQUEOUS MEDIA USING IONIC LIQUIDS

The present invention relates to a method for extracting metal and/or metalloid ions from an aqueous medium, comprising the steps of: a) mixing the aqueous medium with an ionic liquid comprising an aliphatic carboxylate anion having at least one unsaturated carbon-carbon bond, or and/or with a cation comprising at least two amino acids; b) transferring the metal and/or metalloid ions from the aqueous medium to the ionic liquid; c) separating the ionic liquid and the aqueous medium; and d) obtaining the metal and/or metalloid ions from the ionic liquid by at least one method selected from electrochemically reducing the metal and/or metalloid ions, crystallization, and precipitation. Further, the present invention relates to the ionic liquids and their use thereof.

PROCESS FOR PRODUCING FINE MAGNETIC-SUBSTANCE PARTICLE, FINE MAGNETIC-SUBSTANCE PARTICLE OBTAINED BY THE SAME, AND PROCESS FOR PRODUCING MAGNETIC FLUID OR MAGNETIC-SUBSTANCE PRODUCT

A process for producing fine magnetic-substance particles. By the process, monodisperse fine magnetic-substance particles can be produced. The product is self-dischargeable and causes no clogging. The process does not necessitate a high pressure and attains high productivity. At least two fluids are used in the process. At least one of the fluids is a fluid containing at least one raw material for a magnetic substance. At least one of the fluids other than that fluid is a fluid containing at least one precipitant for fine magnetic-substance particles. These fluids are caused to meet each other in a thin-film fluid formed between treatment planes which are disposed face to face so as to be capable of being brought near to or apart from each other and at least one of which rotates with respect to the other. Thus, fine magnetic-substance particles are precipitated in that thin-film fluid to obtain fine magnetic-substance particles.

Apparatus and process for preparing crystalline particles

A process for preparing crystalline particles, especially particles of a pharmaceutical or carrier substance suitable for inhalation therapy, in addition to apparatus for the preparation of such particles.

Hydrodynamic cavitation crystallization process

A device and process for crystallizing a compound using hydrodynamic cavitation comprising the steps of mixing at least one stream of a solution of such compound to be crystallized with at least one stream of an anti-solvent and passing the mixed streams at an elevated pressure through a local constriction of flow to create hydrodynamic cavitation thereby causing nucleation and the direct production of crystals.

INOSITOL NICOTINATE CRYSTALLINE FORM A AND PREPARATION METHOD THEREFOR

Provided are an inositol nicotinate crystalline form A and a preparation method therefor. The X-ray powder diffraction analysis, obtained by using Cu-Kα ray measurement, of the inositol nicotinate crystalline form A has obvious characteristic diffraction peaks at least at 2θ values, expressed in degrees, of 7.05, 7.41, 9.74, 17.80, 19.86, 23.57, 25.48 and 26.20 with an error range of +/−0.2°. The preparation method is one of or a mixed crystallization method of two or more of an evaporation crystallization method, a cooling crystallization method or an anti-solvent crystallization method. The process thereof is simple and easy to operate, and has more selectivity; the inositol nicotinate crystalline form A can be prepared by various methods, and the prepared product has a good crystallization degree and high chemical stability; and the inositol nicotinate crystalline form A prepared by the present method does not have the problem that a residual solvent is out-of-limit. 1. An crystal form A of inositol nicotinate , wherein X-ray powder diffraction analysis of the crystal form A obtained using Cu-Kα ray measurement , with an error range of ±0.2° , has an obvious characteristic diffraction peak at least at 7.05 , 7.41 , 9.74 , 17.80 , 19.86 , 23.57 , 25.48 and 26.20 of 2θ value expressed as degrees , with an error range of ±0.2°.2. The crystal form A of inositol nicotinate of claim 1 , wherein the X-ray powder diffraction of crystal form A expressed as 2θ value degrees has an obvious characteristic diffraction peak at diffraction angles of 7.05 claim 1 , 7.41 claim 1 , 9.74 claim 1 , 10.16 claim 1 , 11.26 claim 1 , 12.75 claim 1 , 17.80 claim 1 , 19.86 claim 1 , 20.97 claim 1 , 23.57 claim 1 , 25.48 and 26.20 claim 1 , 26.58 claim 1 , with an error range of ±0.2°.4. The crystal form A of inositol nicotinate of claim 1 , wherein the X-ray powder diffraction pattern of the crystal form A is essentially as shown in .5. The crystal form A of inositol nicotinate of claim 1 ...

Apparatus and method for producing dispersions and solids

In order to create an apparatus with which solvent/nonsolvent precipitations may be carried out in such a way as to produce particles that are as small as possible and largely free of Ostwald ripening in the dispersion being formed, it is suggested according to the invention that the educt outlet be followed by a spray-drier unit and that a feedback control system be provided to optimize and maintain the operating parameters for the spray-drier unit.

Production of crystalline materials by using high intensity ultrasound

A crystalline material sufficiently pure for use in pharmaceuticals may be made by forming a saturated solution of the material changing the temperature of the solution so it becomes supersaturated, and briefly subjecting the solution to irradiation by high intensity ultrasound, before allowing the solution to cool gradually without further irradiation. The ultrasound may be applied using a vessel with an array of ultrasonic transducers attached to a wall, so each transducer radiates no more than 3 W/cm2 yet the power dissipation within the vessel is between 25 and 150 W/litre. This method can reduce the metastable zone width to less than 10 K. There is no erosion of the wall and consequently no formation of small particles of metal. It is applicable for example to aspartame, and to amino acids.

Process for carrying out crystallization

The present invention is directed to a crystallization process and apparatuses for such processes. In a first aspect, the process of the invention comprises a step wherein a liquid comprising a solvent and material dissolved therein, is subjected to crystallization conditions in the presence of Dean vortices, which Dean vortices result from said liquid flowing through a channel having at least one curvature. In a second aspect, the invention is directed to a crystallization process, which comprises a step wherein a liquid comprising a solvent, material dissolved therein and heterogeneous particles is subjected to crystallization conditions in the presence of Dean vortices, which Dean vortices result from said liquid flowing through a channel having at least one curvature, wherein said material crystallizes on solid surfaces, in particular on surfaces of the heterogeneous particles present in the feed.

METHOD FOR PRODUCING CRYSTALLINE ACTIVE INGREDIENT PARTICLES

MICROFLUIDIC DEVICE FOR CRYSTALLIZATION AND CHRYSTALLOGRAPHIC ANALYSIS OF MOLECULES

PROCESS FOR MAKING CRYSTALS

СПОСОБ НЕПРЕРЫВНОЙ ПОДГОТОВКИ КРИСТАЛЛОВ МЕТИОНИНА ВЫСОКОЙ НАСЫПНОЙ ПЛОТНОСТИ

FIELD: manufacturing technology.SUBSTANCE: invention relates to a method for the continuous preparation of high bulk density methionine crystals. Process is as follows: mix the solution of the hydrolyzate containing potassium and methionine and the resulting 5-(β-methylmercaptoethyl)hydantoin and a solution of potassium carbonate with an external circulation material from a neutralization crystallizer with a circulation tube and a septum (TsiP) having a gas-phase neutralization section; after cooling, the mixture material is introduced into the liquid distributor of the neutralization area in the upper part of the crystallizer and is sprayed in the form of drops or thin streams of liquid into the zone of contact of gas and liquid for carrying out the neutralization reaction, after which the fall of the neutralization solution in a natural way to the crystallization region in the lower part, where it mixes with the material in the said region; provide the cultivation of the mixture on small crystals in the system for the formation of crystals, having particles of larger diameter, and at the same time new crystallization centers are formed; in the deposition zone in the middle part of the crystallization region, crystals with particles of larger diameter are deposited in the pipe for wet elutriation of crystals, while small crystals circulate with the material of external circulation, and part of the material of external circulation is used for wet elutriation of crystals in the pipe for wet elutriation of crystals, while the other part of this material is mixed with a solution of hydrolyzate; and the crystals in the nozzle for wet elutriation of crystals are subjected to separation, washed and dried to obtain a product of methionine high bulk density.EFFECT: continuous preparation of methionine crystals of high bulk density.12 cl, 1 dwg, 5 ex, 1 tbl РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2 678 585 C2 (51) МПК C07C 323/58 (2006.01) C07C 319/28 (2006.01) B01D 9/02 ( ...

Patent RU2019133577A3

ВУ“? 2019133577” АЗ Дата публикации: 30.07.2021 Форма № 18 ИЗПМ-2011 Федеральная служба по интеллектуальной собственности Федеральное государственное бюджетное учреждение 5 «Федеральный институт промышленной собственности» (ФИПС) ОТЧЕТ О ПОИСКЕ 1. . ИДЕНТИФИКАЦИЯ ЗАЯВКИ Регистрационный номер Дата подачи 2019133577/04(066252) 28.03.2018 РСТ/ЕР2018/057875 28.03.2018 Приоритет установлен по дате: [ ] подачи заявки [ ] поступления дополнительных материалов от к ранее поданной заявке № [ ] приоритета по первоначальной заявке № из которой данная заявка выделена [ ] подачи первоначальной заявки № из которой данная заявка выделена [ ] подачи ранее поданной заявки № [Х] подачи первой(ых) заявки(ок) в государстве-участнике Парижской конвенции (31) Номер первой(ых) заявки(ок) (32) Дата подачи первой(ых) заявки(ок) (33) Код страны 1. 17163826.5 30.03.2017 ЕР Название изобретения (полезной модели): [Х] - как заявлено; [ ] - уточненное (см. Примечания) ТВЕРДАЯ ФОРМА (5)-[2-хлор-4-фтор-5-(7-морфолин-4-илхиназолин-4-ил)фенил]-(6- метокси-пиридазин-3-ил)метанола Заявитель: МЕРК ПАТЕНТ ГМБХ, РЕ 2. ЕДИНСТВО ИЗОБРЕТЕНИЯ [Х] соблюдено [ ] не соблюдено. Пояснения: см. Примечания 3. ФОРМУЛА ИЗОБРЕТЕНИЯ: [Х] приняты во внимание все пункты (см. п см. Примечания [ ] приняты во внимание следующие пункты: [ ] принята во внимание измененная формула изобретения (см. Примечания) 4. КЛАССИФИКАЦИЯ ОБЪЕКТА ИЗОБРЕТЕНИЯ (ПОЛЕЗНОЙ МОДЕЛИ) (Указываются индексы МПК и индикатор текущей версии) (070 403/10 (2006.01) 5. ОБЛАСТЬ ПОИСКА 5.1 Проверенный минимум документации РСТ (указывается индексами МПК) С07р 405/14, С07О 403/10, С07О 401/14, Аб1К 31/506, Аб1Р 35/00 5.2 Другая проверенная документация в той мере, в какой она включена в поисковые подборки: 5.3 Электронные базы данных, использованные при поиске (название базы, и если, возможно, поисковые термины): Езрасепе, Рабеагсв 6. ДОКУМЕНТЫ, ОТНОСЯЩИЕСЯ К ПРЕДМЕТУ ПОИСКА Кате- Наименование документа с указанием (где необходимо) частей, Относится к гория* ...

КРИСТАЛЛИЧЕСКАЯ ФОРМА МАЛЕАТА КОНДЕНСИРОВАННОГО ПИРИДИНОВОГО ПРОИЗВОДНОГО И СПОСОБЫ ЕЕ ПРИМЕНЕНИЯ

РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2018 106 101 A (51) МПК C07D 487/04 (2006.01) C07D 401/14 (2006.01) A61K 31/437 (2006.01) A61P 35/00 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ЗАЯВКА НА ИЗОБРЕТЕНИЕ (21)(22) Заявка: 2018106101, 20.07.2016 (71) Заявитель(и): БЕТТА ФАРМАСЬЮТИКАЛЗ КО., ЛТД (CN) Приоритет(ы): (30) Конвенционный приоритет: 20.07.2015 CN PCT/CN2015/084414 (85) Дата начала рассмотрения заявки PCT на национальной фазе: 20.02.2018 (86) Заявка PCT: (87) Публикация заявки PCT: WO 2017/012539 (26.01.2017) A Адрес для переписки: 123242, Москва, Кудринская пл., 1, а/я 35, "Михайлюк, Сороколат и партнеры-патентные поверенные" R U (57) Формула изобретения 1. Кристаллическая форма соединения формулы I, A 2 0 1 8 1 0 6 1 0 1 (54) КРИСТАЛЛИЧЕСКАЯ ФОРМА МАЛЕАТА КОНДЕНСИРОВАННОГО ПИРИДИНОВОГО ПРОИЗВОДНОГО И СПОСОБЫ ЕЕ ПРИМЕНЕНИЯ 2 0 1 8 1 0 6 1 0 1 CN 2016/090613 (20.07.2016) R U (43) Дата публикации заявки: 20.08.2019 Бюл. № 23 (72) Автор(ы): ХУ Шаоцзин (CN), ЛУН Вэй (CN), ЧЖОУ Люфэн (CN), СЮЙ Чжигоу (CN), ВАН Фэй (CN) Формула I, где ее порошковая рентгенограмма характеризуется характеристическими пиками при дифракционных углах 2θ при значениях 8,6°±0,2°, 16,5°±0,2° и 26,5°±0,2°. 2. Кристаллическая форма по п. 1, где ее порошковая рентгенограмма характеризуется характеристическими пиками при дифракционных углах 2θ при значениях 8,6°±0,2°, 15,8°±0,2°, 16,5°±0,2°, 19,5°±0,2°, 20,2°±0,2° и 26,5°±0,2°. 3. Кристаллическая форма по любому из пп. 1-2, где ее порошковая рентгенограмма характеризуется характеристическими пиками при дифракционных углах 2θ при значениях 8,6°±0,2°, 10,5°±0,2°, 15,8°±0,2°, 16,5°±0,2°, 19,5°±0,2°, 20,2°±0,2°, 23,6°±0,2°, 26,5°±0,2° и 29,1°±0,2°. Стр.: 1 2 0 1 8 1 0 6 1 0 1 R U A Стр.: 2 2 0 1 8 1 0 6 1 0 1 Формула II, с малеиновой кислотой в реакционной среде на основе этилацетата в стеклянном реакторе при комнатной температуре, центрифугирование и высушивание в течение ночи под вакуумом при комнатной температуре с ...

СПОСОБЫ ПОЛУЧЕНИЯ ФОСФОРОРГАНИЧЕСКИХ СОЕДИНЕНИЙ

Particle formation methods and their products

Dota synthesis

Crystallisation method and apparatus

Particulate products

Novel apparatus and process

PROCEDURE FOR THE SOLIDIFICATION, WITH WHICH AN ANTI SOLVENT IS USED

Particle formation methods and their products

Method for extracting silica

Provided are methods of extracting silica and optionally lignin from an organic material, which includes adding a first acid to a liquids fraction separated from the organic material after treatment thereof with an alkali so as to facilitate at least partial precipitation of silica therefrom and then separating precipitated silica from the liquids fraction. The methods provided herein may optionally include adding a second acid to the liquids fraction so as to facilitate at least partial precipitation of lignin therefrom. In one form, the method further includes contacting the aforementioned liquids fraction with an ion-exchanger so as to facilitate at least partial substitution of a first cation of the liquids fraction with a second cation of the ion-exchanger, such that the liquids fraction is then suitable as a liquid fertilizer. Silica and lignin precipitates and a liquid fertilizer produced by the present methods are also provided.

Process for making sterile aripiprazole of desired mean particle size

A process is provided for making sterile aripiprazole having an average particle size less than 100 microns but preferably greater than 25 microns employing an impinging jet crystallization procedure. The resulting bulk aripiprazole of desired particle size may be used to form a sterile freeze-dried aripiprazole formulation, which upon constitution with water and intramuscular injection releases aripiprazole over a period of at least about one week and up to about eight weeks.

RESINOUS COMPOUND CRYSTALLIZATION USING NON-POLAR SOLVENT SEQUENCE

A resin containing a desirable compound is extracted from plant material and dissolved in a volatile non-polar solvent. The solvent is evaporated, cooling the solution and increasing the saturation level of the compound in the solution. A second volatile non-polar solvent, in which the compound is less soluble, is then added to the solution and evaporated. This again cools the solution and increases the saturation level until the compound has started to crystallize. The crystals are then filtered and rinsed. Crystallization is more rapid compared to traditional techniques. The resin is obtained from the plant material using an extraction solvent to form a solution, which is then floated above an immiscible liquid, where it is drawn off through a screen and the extraction solvent evaporated. 1. A method for crystallizing a compound from a resin , comprising:mixing a first non-polar solvent with the resin to form a solution;evaporating the first non-polar solvent from the solution;then, mixing a second non-polar solvent with the solution, wherein the compound has a lower solubility in the second non-polar solvent than in the first non-polar solvent;removing the second non-polar solvent from the solution to cause a temperature of the solution to drop and the compound to form crystals.2. The method of claim 1 , wherein the first non-polar solvent has a higher boiling point than the second non-polar solvent.3. The method of claim 1 , wherein the first non-polar solvent is miscible with the second non-polar solvent.4. The method of claim 1 , wherein the first non-polar solvent is butane and the second non-polar solvent is propane.5. The method of claim 1 , wherein the first non-polar solvent is evaporated by pumping off the first non-polar solvent in its gaseous phase.6. The method of claim 1 , wherein the solution is maintained at a temperature of 0-20° C. and between a pressure of 0-140 kPa while evaporating the first non-polar solvent from the solution.7. The method of ...

PROCESSES FOR PRODUCING ORGANOPHOSPHOROUS COMPOUNDS

The present invention relates to processes for producing organophosporous compositions having low acid content as well as processes for reprocessing partially degraded organophosporous compositions that contain high levels of phosphorous acid. In one embodiment, a process comprises: (a) receiving a solid organophosphite compound that has been recrystallized or triturated, wherein the solid organophosphite compound comprises phosphorous acid; (b) dissolving the solid organophosphite compound in a an aromatic hydrocarbon solvent in the absence of water and free amine, wherein the hydrocarbon solvent comprises an aromatic hydrocarbon, a saturated aliphatic hydrocarbon, or a mixture thereof; and (c) removing undissolved phosphorous acid from the solution, wherein the acid content of the organophosphite following step (c) is 30 ppm or less. 1. A process comprising: (a) receiving a solid organophosphite compound that has been recrystallized or triturated , wherein the solid organophosphite compound comprises phosphorous acid; (b) dissolving the solid organophosphite compound in a hydrocarbon solvent , wherein the hydrocarbon solvent comprises an aromatic hydrocarbon , a saturated aliphatic hydrocarbon , or a mixture thereof; and (c) removing undissolved phosphorous acid from the solution , wherein the acid content of the organophosphite following step (c) is 30 ppm or less.2. The process of claim 1 , wherein the undissolved phosphorous acid is removed by filtration.3. The process of claim 1 , wherein the undissolved phosphorous acid is removed by centrifugation.4. The process of claim 1 , wherein the acid content of the organophosphite following step (c) is 10 ppm or less.5. The process of claim 1 , wherein the acid content of the organophosphite following step(c) is 5 ppm or less.6. The process of claim 1 , further comprising (d) concentrating the organophosphite in hydrocarbon solution; (e) combining the concentrated organophosphite in hydrocarbon solution with an anti- ...

PROCESSES FOR PRODUCING ORGANOPHOSPHOROUS COMPOUNDS

The present invention relates to processes for producing organophosporous compositions having low acid content as well as processes for reprocessing partially degraded organophosporous compositions that contain high levels of phosphorous acid. In one embodiment, a process comprises: (a) receiving a solid organophosphite compound that has been recrystallized or triturated, wherein the solid organophosphite compound comprises phosphorous acid; (b) dissolving the solid organophosphite compound in an organic solvent; (c) treating the solution with a weakly basic adsorbent; and (d) collecting the treated organophosphite solution, wherein the acid content of the organophosphite following step (d) is 30 ppm or less. 1. A process comprising: (a) receiving a solid organophosphite compound that has been recrystallized or triturated , wherein the solid organophosphite compound comprises phosphorous acid; (b) dissolving the solid organophosphite compound in an organic solvent; and (c) treating the solution with a weakly basic adsorbent; and (d) collecting the treated organophosphite solution , wherein the acid content of the organophosphite following step (d) is 30 ppm or less.2. The process of claim 1 , wherein the weakly basic adsorbent comprises a metal oxide claim 1 , a metal carbonate claim 1 , or an anionic clay having an effective pKa of less than 12 or a weakly basic ion exchange resin.3. The process of claim 2 , wherein the weakly basic adsorbent comprises a weakly basic ion exchange resin claim 2 , and the weakly basic ion exchange resin comprises at least 10 equivalents of a basic moiety per mole of acid in the organophosphite solution.4. The process of claim 1 , wherein the solid organophosphite compound is dissolved in the organic solvent in the absence of free amine.5. The process of claim 1 , wherein the solvent comprises toluene claim 1 , xylenes claim 1 , diethyl ether claim 1 , dichloromethane claim 1 , ethyl acetate claim 1 , butyraldehyde claim 1 , ...

Synthesis of ammonium dinitramide (adn)

The invention concerns a method for making ammonium dinitramide from guanylurea dinitramide in one single process step. Guanylurea dinitramide is reacted with an ammonium sulfate in a reaction solution comprising water and acetone and an ion exchange gives ammonium dinitramide. By using acetone the yield is increased compared to known processes as formed guanylurea sulfate is poorly soluable in a water-acetone solution and precipitates, while guanylurea dinitramide has higher solubility in the solution than in only water. The guanylurea sulfate precipitate formed in the reaction solution that contains acetone is less sticky than if formed in water or in a water-alcohol solution and therefore easier to filter off. The use of acetone also allows lower process temperatures to be used than in previously known methods for producing guanylurea dinitramide. Conclusively, the method gives a higher yield, demands considerable smaller amounts of solvent and allows lower process temperatures to be used than in any formerly known process.

Compositions that contain lipophilic plant material and surfactant, and related methods

Described are liquid compositions that contain a desired (e.g., extracted) plant material such as cannabinoid, terpene, terpenoid, or the like, contained, e.g., dissolved, suspended, or emulsified, in the liquid, which contains surfactant; methods of preparing these types of liquid compositions; and methods of processing this type of liquid composition to collect, isolate, concentrate, or purify a desired target material contained in the liquid composition.

Process Scheme To Improve Divalent Metal Salts Removal From Mono Ethylene Glycol (MEG)

A MEG reclamation process includes the step of increasing above 2,000 ppm the divalent metal salts concentration of a rich (wet) MEG feed stream flowing into a precipitator. The increasing step includes routing a salts-saturated MEG slipstream from the flash separator it to the precipitator. The slipstream may be mixed with a fresh water feed stream, a portion of the rich MEG feed stream, or some combination of the two. The rich MEG feed stream also may be split into two streams, with a portion of the stream being heated and routed to the flash separator and the other portion being combined as above with the removed slipstream. The process can be performed on the slipstream after dilution and prior to entering the precipitator or after being loaded into the precipitator. Removal of the insoluble salts may be done in either a batch or continuous mode.

PROCESS FOR THE PREPARATION OF D-GLUCITOL, 1,5-ANHYDRO-1-C-[4-CHLORO-3-[[4-[[(3S)-TETRAHYDRO-3-FURANYL] OXY]PHENYL] METHYL] PHENYL]-, (1S) AND ITS CRYSTALLINE FORMS THEREOF

The present invention relates to process for the preparation of D-glucitol, 1,5-anhydro-1-C-[4-chloro-3-[[4-[[(3S)-tetrahydro-3-furanyl]oxy]phenyl] methyl]phenyl]-, (1S) formula-1 and its crystalline forms thereof. 2. The process according to claim 1 , wherein claim 1 , in step-a) claim 1 , the suitable thiol reagent is thiol or dithiol alcohol which is selected from decanethiol claim 1 , dodecane thiol claim 1 , cyclohexane thiol claim 1 , cyclopentane thiol claim 1 , cyclo butane thiol claim 1 , thiophenol claim 1 , methanethiol claim 1 , ethanethiol claim 1 , 1-propanethiol claim 1 , 2-propanethiol claim 1 , n-butanethiol claim 1 , tert-butanthiol claim 1 , furan-2-ylmethanethiol claim 1 , ethandithiol claim 1 , 1 claim 1 ,2-propanedithiol claim 1 , 1 claim 1 ,3-propanedithiol claim 1 , 1 claim 1 ,3-butanedithiol claim 1 , 1 claim 1 ,4-butanedithiol; the suitable Lewis acid is selected from AlCl claim 1 , AlBr claim 1 , BCl claim 1 , TiCl claim 1 , FeCland ZnCl.3. The process according to claim 1 , wherein claim 1 , in step-b) claim 1 , the suitable base is selected from “alkali metal hydroxides” such as lithium hydroxide claim 1 , sodium hydroxide claim 1 , potassium hydroxide and the like; “alkali metal carbonates” such as sodium carbonate claim 1 , potassium carbonate claim 1 , lithium carbonate and the like; “alkali metal bicarbonates” such as sodium bicarbonate claim 1 , potassium bicarbonate claim 1 , lithium bicarbonate and the like; “alkali metal hydrides” such as sodium hydride claim 1 , potassium hydride claim 1 , lithium hydride and the like; “alkali metal alkoxides” such as sodium methoxide claim 1 , sodium ethoxide claim 1 , sodium tert-butoxide claim 1 , potassium methoxide claim 1 , potassium ethoxide claim 1 , potassium tert-butoxide and the like.4. The process according to claim 1 , wherein claim 1 , in step-a) and step-b) claim 1 , the suitable solvent is selected from alcohol solvents such as methanol claim 1 , ethanol claim 1 , n-propanol ...

Methods of isolating phenols from phenol-containing media

Methods of isolating phenols from phenol-containing media. The methods include combining a phospholipid-containing composition with the phenol-containing medium to generate a combined medium, incubating the combined medium to precipitate phenols in the combined medium and thereby form a phenol precipitate phase and a phenol-depleted phase, and separating the phenol precipitate phase and the phenol-depleted phase. The methods can further include extracting phenols from the separated phenol precipitate phase. The extracting can include mixing the separated phenol precipitate phase with an extraction solvent to solubilize in the extraction solvent at least a portion of the phenols originally present in the phenol precipitate phase.

Method and system for refining long chain dicarboxylic acid

The present disclosure provides a system for refining long chain dicarboxylic acid, comprising: a first membrane filtration unit, for a first membrane filtration of a long chain dicarboxylic acid fermentation broth or a treated liquid therefrom; a first decolorization unit, for carrying out a first decolorization treatment to the filtrate obtained after the membrane filtration; a first acidification/crystallization unit, for carrying out a first acidification/crystallization of a filtrate obtained after the membrane filtration to give a solid-liquid mixture; a first separation unit, for a solid-liquid separation of the solid-liquid mixture; a drying unit, for drying the solid separated by the separation unit to give a first solid. By using the refining system according to the present disclosure, the purity of the obtained product is high, and the disadvantages such as poor quality of the product obtained by crystallization from a solvent and environment pollution caused by a solvent can be overcome.

Process for the Preparation of Amorphous Idelalisib and its Premix

Processes for the preparation of amorphous idelalisib are provided. Processes for the preparation of a premix of amorphous idelalisib are also provided. 1. A method of producing amorphous idelalisib , comprising the steps of:a) dissolving idelalisib in a solvent;b) adding an anti-solvent; andc) isolating amorphous idelalisib.2. The method of claim 1 , wherein the solvent is selected from the group consisting of methanol claim 1 , ethanol claim 1 , n-propanol claim 1 , isopropanol claim 1 , n-butanol claim 1 , t-butanol claim 1 , formic acid claim 1 , dimethyl sulfoxide claim 1 , dimethylformamide claim 1 , dimethylacetamide claim 1 , 2-methyl tetrahydrofuran claim 1 , N-methyl-2-pyrrolidone claim 1 , and mixtures thereof.3. The method of claim 1 , wherein the anti-solvent is selected from the group consisting of water claim 1 , dichloromethane claim 1 , and mixtures thereof.4. The method of claim 1 , wherein the adding of the anti-solvent results in the formation of a precipitate.5. The method of claim 1 , wherein the isolating step is achieved by filtering and drying the precipitate claim 1 , distillation claim 1 , spray drying claim 1 , lyophilization claim 1 , or agitated thin film drying.6. A process for the preparation of a premix of amorphous idelalisib claim 1 , comprising the steps of:a) dissolving idelalisib in an organic solvent;b) adding a pharmaceutically acceptable excipient; andc) removing the solvent to isolate a premix of amorphous idelalisib.7. The process according to claim 6 , wherein the organic solvent is an alcohol.8. The process according to claim 7 , wherein the alcohol is selected from the group consisting of methanol claim 7 , ethanol claim 7 , isopropanol claim 7 , n-butanol claim 7 , and mixtures thereof.9. The process according to claim 6 , wherein the pharmaceutically acceptable excipient is selected from the group consisting of polyols claim 6 , polymers claim 6 , and mixtures thereof.10. The process according to claim 9 , wherein the ...

HYDRATE OF 2-ISOPROPOXY-5-METHYL-4-(PIPERIDIN-4-YL) ANILINE DIHYDROCHLORIDE, PREPARATION METHOD AND USE OF THE SAME

The present invention relates to 2-isopropoxy-5-methyl-4-(piperidin-4-yl) aniline dihydrochloride monohydrate and a preparation method of the same. The 2-isopropoxy-5-methyl-4-(piperidin-4-yl) aniline dihydrochloride monohydrate has a very good crystal form and is well suitable for recrystallization purification; further, the effect of impurity removal effect is very good, and any single impurity can be controlled less than 0.1%. 2. A method of preparing 2-isopropoxy-5-methyl-4-(piperidin-4-yl)aniline dihydrochloride monohydrate , comprising:dissolving 4-(5-isopropoxy-2-methyl-4-nitro-phenyl)pyridine in an alcoholic solvent, and reducing by hydrogenating reduction via a noble metal catalyst to obtain 2-isopropoxy-5-methyl-4-(piperidin-4-yl) aniline free base; andreacting the 2-isopropoxy-5-methyl-4-(piperidin-4-yl) aniline free base with an alcoholic solution of hydrochloric acid or hydrogen chloride.3. The method according to claim 2 , wherein alcohols present in the alcoholic solvent or the alcoholic solution are independently one or more selected from the group consisting of methanol claim 2 , ethanol claim 2 , propanol claim 2 , isopropanol claim 2 , butanol claim 2 , isobutanol claim 2 , pentanol claim 2 , 2-pentanol and hexanol.4. The method according to claim 1 ,wherein the decomposition point of hydrate of the 2-isopropoxy-5-methyl-4-(piperidin-4-yl)aniline dihydrochloride monohydrate is higher than 130° C., and the weight loss thereof by drying at 120° C. is not more than 1%, as determined in thermogravimetric analysis; andwherein the decomposition point of the 2-isopropoxy-5-methyl-4-(piperidin-4-yl)aniline dihydrochloride monohydrate is more than 230° C., and the weight loss thereof by drying at 170° C. is not more than 7%, as determined in thermogravimetric analysis.5. A crystal form A of 2-isopropoxy-5-methyl-4-(piperidin-4-yl)aniline dihydrochloride monohydrate claim 1 , wherein the X-ray powder diffraction pattern thereof exhibits characteristic peaks ...

Novel Process for the Preparation of Tavaborole, Its Novel Polymorphic Forms and the Polymorphs Thereof

The invention relates to novel process for preparation of Tavaborole. The invention also relates to novel polymorphic forms of Tavaborole and process for preparation of those polymorphic forms. The invention also relates to process for purification of Tavaborole to obtain the Tavaborole in significantly high yield and substantially pure form. 1. A process for preparation of a crystalline form of Tavaborole comprising the steps of:(d) contacting Tavaborole with a solvent or mixture of solvents;(e) heating the solvent or solvents mixture with Tavaborole to reflux; and 'wherein the solvent or solvents mixture can be selected from water, methanol, Ethanol, Isopropyl alcohol, Methyl tertiary butyl alcohol, Toluene, acetone Tetrahydrofuran, Ethyl acetate, dichloromethane, acetonitrile, methyl tertiary butyl ether or mixtures thereof; and', '(f) precipitating Tavaborole from solvent or solvents mixture by using conventional techniques viz. slow or fast cooling, addition of crystallization solvent, drying at atmospheric or reduced pressure, so as to obtain the desired crystalline form of Tavaborole;'}wherein the crystalline form of Tavaborole produced by the process is any of crystalline forms Form-I, Form-II, Form-III, Form-IV and Form-V, the crystalline forms are characterized by XRPD peaks patterns as depicted in Figure-1, Figure-3, Figure-4, Figure-5 and Figure-6 respectively.2. The crystalline Form I of Tavaborole as claimed in claim 1 , characterized by X-ray powder diffraction (XRPD) pattern comprising one or more of the reflections at value 6.30 claim 1 , 12.66 and 25.5±0.2 degrees 2 theta (2θ°) and which has X-ray powder diffraction pattern as shown in .3. The crystalline Form I of Tavaborole as claimed in claim 2 , further characterized by XRPD pattern comprising one or more of the reflections at value: 5.70 claim 2 , 11.43 claim 2 , 14.25 claim 2 , 14.83 claim 2 , 16.33 claim 2 , 20.31 claim 2 , 26.23 claim 2 , 26.98 claim 2 , 28.84 claim 2 , 30.95 claim 2 , 32. ...

METHODS FOR CONTROLLING CRYSTALLIZATION BASED ON TURBIDITY AND SYSTEMS THEREFOR

Methods and systems for forming crystallized products from solutions. Such a method includes depositing an input material in a solvent mixture comprising a solvent and an anti-solvent, increasing the temperature of the solvent mixture with the input material therein to an elevated temperature for a period of time sufficient to fully dissolve the input material in the solvent mixture to form a solution of the material, and performing a series of temperature cycles on the solution to produce a crystallized product from the material in the solution. The solution is alternated between heating cycles and cooling cycles based on the turbidity of the solution, and the solution is filtered to remove and collect the crystallized product therefrom. 1. A method comprising:depositing an input material in a solvent mixture comprising a solvent and an anti-solvent;increasing the temperature of the solvent mixture with the input material therein to an elevated temperature for a period of time sufficient to fully dissolve the input material in the solvent mixture to form a solution of the material;performing a series of temperature cycles on the solution to produce a crystallized product from the material in the solution, wherein the solution is alternated between heating cycles and cooling cycles based on the turbidity of the solution; andfiltering the solution to remove and collect the crystallized product therefrom.2. The method of claim 1 , wherein the turbidity of the solution is continuously determined using one or more in-line process analytical technology (PAT) tools.3. The method of claim 1 , wherein the turbidity of the solution is continuously determined using image-based analysis.4. The method of claim 3 , wherein the image-based analysis is performed with a probe-based video microscope used to continuously capture high resolution images of the solution.5. The method of claim 1 , further comprising initiating a heating cycle in response to the turbidity reaching or ...

Crystal of reduced glutathione

The present invention provides a crystal of reduced glutathione that is stable, and is easy to process, and a method for producing the crystal. According to the present invention, a crystal of a metal salt of reduced glutathione is produced by suspending an amorphous solid of a metal salt of reduced glutathione in a hydrophobic organic solvent, and adding water to the resulting suspension to precipitate a crystal of a metal salt of reduced glutathione.

CANNABINOID PROCESSING METHODS AND SYSTEMS

A system and method for crystallization and pelleting of a cannabinoid, including cannabidiol (CBD). 1245-. (canceled)246. A method for decarboxylating and crystallizing a cannabinoid comprising providing a cannabinoid extract comprising a cannabinoid to a heat transfer screw at a sufficient temperature;moving the heated cannabinoid extract through the heat transfer screw;introducing a foaming agent to produce a cannabinoid foam;extruding the heated cannabinoid foam into a vessel and passing an anti-solvent at a temperature of −20° C. to 20° C. over the heated cannabinoid foam forming a cannabinoid crystal; andrecovering the cannabinoid crystal.247. The method of claim 246 , wherein the foaming agent is a blowing agent.248. The method of claim 247 , wherein the foaming agent is carbon dioxide (CO) claim 247 , pentane claim 247 , butane claim 247 , chlorofluorocarbons claim 247 , or a mixture thereof.249. The method of claim 246 , wherein the foaming agent is carbon dioxide (CO) produced in situ by decarboxylation of a cannabinoid acid.250. The method of claim 246 , wherein the anti-solvent is pentane claim 246 , butane claim 246 , propane claim 246 , or hexane.251. The method of claim 246 , wherein the anti-solvent extracts terpenes from the cannabinoid foam.252. The method of claim 246 , wherein the cannabinoid extract is provided by means of spraying claim 246 , pouring claim 246 , injection claim 246 , or a combination thereof.253. The method of claim 246 , wherein the cannabinoid crystals are substantially free of lipids.254. The method of claim 246 , wherein the method further comprises collecting the terpenes.255. A method for pelletizing a cannabinoid composition comprising admixing a cannabinoid composition and a binding agent to form a cannabinoid-binding agent mixture.256. The method of claim 255 , wherein the binding agent is a food-grade binding agent.257. The method of claim 255 , wherein the binding agent is a polysaccharide claim 255 , gums claim 255 ...

PLINABULIN COMPOSITIONS

Disclosed herein are plinabulin polymorphs, compositions, their use and preparation as therapeutic agents. In particular, some embodiments relate to plinabulin monohydrate in a crystalline form. 1. A plinabulin monohydrate.2. The plinabulin monohydrate of in crystalline form.3. The plinabulin monohydrate of claim 2 , exhibiting an X-ray powder diffraction pattern comprising at least three characteristic peaks selected from the group consisting of peaks at approximately 8.1° claim 2 , 13.1° claim 2 , 16.3° claim 2 , 23.9° claim 2 , 24.2° claim 2 , 24.5° claim 2 , and 26.6° 2θ.4. The plinabulin monohydrate of claim 2 , exhibiting an X-ray powder diffraction pattern comprising at least peaks at approximately 8.1° claim 2 , 13.1° claim 2 , 16.3° claim 2 , 23.9° claim 2 , 24.2° claim 2 , 24.5° claim 2 , and 26.6° 2θ.5. The plinabulin monohydrate of claim 2 , exhibiting an X-ray powder diffraction pattern comprising at least peaks at approximately 8.1° claim 2 , 13.1° claim 2 , 16.1° claim 2 , 16.3° claim 2 , 19.8° claim 2 , 22.9 claim 2 , 23.9 claim 2 , 24.2 claim 2 , 24.5 claim 2 , 26.6 claim 2 , and 29.3° 2θ.6. The plinabulin monohydrate of claim 2 , wherein the crystalline form has a melting point of about 267° C.7. The plinabulin monohydrate of claim 1 , having a differential scanning calorimetry thermogram with endothermic peaks at about 141° C. and about 267° C.8. A plinabulin composition claim 1 , comprising more than about 50% by weight of the plinabulin monohydrate of any one of to claim 1 , based on the total weight of the composition.9. The composition of claim 8 , comprising more than about 75% by weight of the plinabulin monohydrate claim 8 , based on the total weight of the composition.10. The composition of claim 8 , comprising more than about 90% by weight of the plinabulin monohydrate claim 8 , based on the total weight of the composition.11. The composition of claim 8 , comprising more than about 95% by weight of the plinabulin monohydrate claim 8 , ...

Continuous Production of Particles

The present invention discloses a method to continuously manufacture micro- and/or nanoparticles of single component particles or multi-component particles such as particulate amorphous solid dispersions or particulate co-crystals. The continuous method comprises the steps of 1. preparing a first solution comprising at least one component and at least one solvent and a second solution comprising at least one anti-solvent of the at least one component comprised in the first solution, 2. mixing said first solution and said second solution by means of microfluidization to produce a suspension by precipitation or co-precipitation, 3. feeding said suspension to a filtration system to obtain a concentrate stream, 4. feeding said concentrate stream to a spray dryer, 5. atomizing said concentrate stream using at least one atomization nozzle, 6. drying said atomized concentrate stream to obtain particles, and 7. collecting said particles. Single component particles or multi-component particles, particulate amorphous solid dispersions, particulate co-crystals and pharmaceutical compositions are also disclosed.

PLINABULIN COMPOSITIONS

Disclosed herein are plinabulin polymorphs, compositions, their use and preparation as therapeutic agents. In particular, some embodiments relate to plinabulin monohydrate in a crystalline form. 1. A plinabulin monohydrate. This application is a continuation of U.S. application Ser. No. 15/741635 filed on Jan. 3, 2018, which is the U.S. National Phase of International Application No. PCT/US2016/041773 entitled PLINABULIN COMPOSITIONS, filed Jul. 11, 2016 and published on Jan. 19, 2017 as WO 2017/011399, which claims the benefit of U.S. Provisional Application No. 62/191,990, filed Jul. 13, 2015, the disclosure of which are incorporated herein by reference in their entireties.The present invention relates to the fields of chemistry and medicine. More particularly, the present invention relates to forms and compositions of plinabulin and their preparation.Plinabulin is a synthetic analog of diketopiperazine phenylahistin (halimide) discovered from marine and terrestrial sp. Plinabulin is structurally different from colchicine and its combretastatin-like analogs (eg, fosbretabulin) and binds at or near the colchicine binding site on tubulin monomers. Previous studies showed that plinabulin induced vascular endothelial cell tubulin depolymerization and monolayer permeability at low concentrations compared with colchicine and that it induced apoptosis in Jurkat leukemia cells. Studies of plinabulin as a single agent in patients with advanced malignancies (lung, prostate, and colon cancers) showed a favorable pharmacokinetic, pharmacodynamics, and safety profile.Some embodiments relate to a plinabulin monohydrate.Other embodiments relate to a plinabulin monohydrate in crystalline form.Some embodiments relate to a plinabulin composition having more than about 90% by weight of plinabulin, based on the total weight of the composition.Other embodiments relate to a plinabulin composition having more than about 99% by weight of plinabulin, based on the total weight of molecules ...

NOVEL INDUSTRIAL CRYSTALLIZATION METHOD OF CEFUROXIME SODIUM AND PREPARATION THEREOF

It discloses a new industrial crystallization method of Cefuroxime Sodium, wherein supercritical fluid extraction technology and traditional crystalline technology are combined to realize the recrystallization of Cefuroxime Sodium. Processes such as extraction, adsorption, crystallization and drying are carried out with a supercritical fluid, a solvent, an extraction cell and a crystallization tank to realize the recrystallization of Cefuroxime Sodium under a specific pressure at a specific temperature. 1. A novel industrial crystallization method of Cefuroxime Sodium , characterized in that , combining supercritical fluid extraction and traditional crystallization to realize the recrystallization of Cefuroxime Sodium , preferably dissolving Cefuroxime Sodium in an organic solvent , extracting the organic solvent and the solute in the solution of Cefuroxime Sodium by a supercritical fluid , and changing the solubility of the ingredients in the organic solvent and the supercritical fluid by adjusting the temperature and the pressure to make Cefuroxime Sodium crystallize.2. The method according to claim 1 , characterized in that including Cefuroxime Sodium prepared by the method claim 1 , and a sterile powder for injection containing Cefuroxime Sodium.3. The method according to claim 2 , characterized in that claim 2 , the solution of Cefuroxime Sodium is subjected to supercritical fluid extraction for 5˜20 minutes under a pressure of 15˜40 MPa at a temperature of 40˜60° C. claim 2 , and Cefuroxime Sodium is crystallized and separated from its solution for 20˜40 minutes under a pressure of 0.5˜5 MPa at a temperature of 20˜30° C.4. The method according to claim 3 , characterized in that claim 3 , said solvent for dissolving Cefuroxime Sodium is selected from one of alcohols claim 3 , aldehydes claim 3 , esters claim 3 , ketones claim 3 , ethers claim 3 , water and so on or a mixture thereof claim 3 , an aqueous ethanol is preferable claim 3 , and an aqueous ethanol ...

Recrystallized HI-6 Dimethylsulfate

The present invention is directed at the synthesis and characterization of recrystallized HI-6 dimethylsulfate (DMS). The method can comprise dissolving HI-6 DMS in an alkyl-based glycol and adding an antisolvent to recrystallize HI-6 DMS or dissolving HI-6 DMS in methanol and adding dimethoxy ethane or dimethyl formamide as the antisolvent to recrystallize HI-6 DMS. The recrystallized HI-6 DMS indicates a resistance to moisture absorption and/or a DSC melting point onset (MP Onset) at least at or above 160.0° C. 1. A method for recrystallizing HI-6 DMS comprising:dissolving HI-6 DMS in an alkyl-based glycol and adding an antisolvent to recrystallize HI-6 DMS.2. The method of wherein said alkyl-based glycol comprises ethylene glycol.3. The method of wherein said alkyl-based glycol comprises 1 claim 1 ,2-propane diol.4. The method of wherein said antisolvent is selected from tert-butanol.5. The method of wherein said antisolvent is selected from acetonitrile.6. The method of wherein said antisolvent is selected from ethanol.7. The method of wherein said antisolvent is selected from dimethoxy ethane.8. The method of wherein said alkyl-based glycol comprises 1 claim 1 ,2-propane diol and said recrystallized HI-6 DMS indicates a DSC melting point onset (MP Onset) at least at or above 160.0° C.9. The method of wherein said alkyl-based glycol comprises 1 claim 1 ,2-propane diol and said recrystallized HI-6 DMS indicates a DSC melting point at least at or above 165.0° C.10. The method of wherein said alkyl-based glycol comprises ethylene glycol and said antisolvent comprises tert-butanol.11. The method of wherein said recrystallized HI-6 DMS does not absorb water over a seven-day period under ambient temperature and humidity conditions.12. The method of wherein said alkyl-based glycol comprises 1 claim 1 ,2-propane diol and said antisolvent comprises tert-butanol.13. The method of wherein said recrystallized HI-6 DMS does not absorb water over a seven-day period under ...

EXPERIMENT SYSTEM AND METHOD FOR ACCURATE CONTROLLING OF MACROMOLECULAR CRYSTALLIZATION PROCESS

An experiment system and method for accurate controlling of macromolecular crystallization process. The system has a platform-equipped horizontal moving slot and channel dedicated backwash module, a droplet adding control module, an observing module, a user observation computer system, and an experimental condition control module. A high-precision movement knob of the x-axis platform and the y-axis platform of the system and the accurate position control of a syringe needle are used to ensure that the macromolecular solution can be added into the correct positions of convex or concave. The crystallization induction period of the target crystal faun is determined by the real-time data of the high-speed microcamera, and the crystal cultivation environment is adjusted in real time. This is simple and easy to operate, high in productivity, can be applied to the conventional experimental replication. 1. An experiment system for accurate controlling of macromolecular crystallization process , wherein the experiment system is a closed space encircled by a shell at ordinary pressure and is mainly composed of a platform-equipped horizontal moving slot and channel dedicated backwash module , a droplet adding control module , an observing module , a user observation computer system , and an experiment condition control module; the platform-equipped horizontal moving slot and channel dedicated backwash module , the droplet adding control module , the observing module and the experiment condition control module are positioned inside the closed space , and the user observation computer system is positioned outside the closed space;the platform-equipped horizontal moving slot and channel dedicated backwash module comprises a platform horizontal moving slot, an x-axis horizontal adjusting mechanism, a y-axis horizontal adjusting mechanism and a high-throughput macromolecular crystal cultivation platform; the high-throughput macromolecular crystal cultivation platform is placed on ...

CONTINUOUS CRYSTALLIZATION METHOD UNDER CONTROL OF MULTISTAGE MEMBRANE

The present invention provides a continuous crystallization method under control of the multistage membrane modules, and belongs to the technical field of crystallization engineering. A crystallization solution is added to a crystallizer, and a stirring apparatus and a temperature control apparatus are started. After the system running stability, the loop of crystallization is started. Meanwhile, the coolant or antisolvent feed liquid loop is also started. The crystallization solution can respectively conduct crystal nucleation, growth and ripening in the multistage membrane modules, and then the crystallization solution is transported into a filter device and a drying apparatus to obtain the final crystal products. The desired crystal products can be obtained by the systematical control of the nucleation and crystal growth through the flow and the temperature of the crystallization solution, coolant or antisolvent feed liquid, and the contact time between two liquid phases. 1. A continuous crystallization method under control of multistage membrane , wherein a continuous crystallization apparatus is composed by two loops;a first loop: a first stirring apparatus is installed in a crystallizer with a jacket; the jacket is connected with a first temperature control apparatus through a pipeline; an outlet of the crystallizer is connected with a lower port of a first membrane module in a membrane module combination successively through a first peristaltic pump, a first rotameter, a first valve, a first thermometer and a first pressure gauge; one path of an upper port of a last membrane module in the membrane module combination is connected with an inlet of the crystallizer through a seventh valve; another path of the upper port of the last membrane module in the membrane module combination is connected with a filter device through a third valve; an upper port of the filter device is connected with an inlet of the crystallizer, and a lower port of the filter device is ...

Novel Process for the Preparation of Tavaborole, Its Novel Polymorphic Forms and the Polymorphs Thereof

The invention relates to novel process for preparation of Tavaborole. The invention also relates to novel polymorphic forms of Tavaborole and process for preparation of those polymorphic forms. The invention also relates to process for purification of Tavaborole to obtain the Tavaborole in significantly high yield and substantially pure form. 3. (canceled)4. The process as claimed in claim 1 , wherein the hydroxyl protecting agent comprises acyl protecting agent selected from the group consisting of acetyl chloride claim 1 , acetic anhydride claim 1 , and benzoyl chloride claim 1 , or Silyl protecting agents selected from the group consisting of trimethyl silyl chloride claim 1 , triethyl silyl chloride claim 1 , and tertiary butyl dimethyl silyl chloride (TBDMSCl).5. (canceled)6. The process as claimed in claim 1 , wherein transition metal catalyzed cross-coupling reaction of step (ii) is carried out in presence of Pd catalyst selected from PdCl(dppf) claim 1 , [PdCldppf]CHCl claim 1 , PdCl(PPh) claim 1 , Pd(PPh) claim 1 , Pd(OAc) claim 1 , [Pddba] claim 1 , [Pd(allyl)Cl] claim 1 , Pd(acac) claim 1 , PhPd(OAc)(PPh)or any Palladium catalyst that generates in situ Pd(O) and combinations thereof claim 1 , or Ni catalyst selected from NiCl(dppp) claim 1 , NiCl(dppf) claim 1 , NiCl(dppe) claim 1 , NiCl.glyme claim 1 , NiBr.glyme claim 1 , NiCl(PPh) claim 1 , NiCl(PCy) claim 1 , Ni(PPh) claim 1 , Ni(PPh) claim 1 , Ni(COD) claim 1 , NiCl claim 1 , NiBror any Nickel catalyst that generates in situ Ni(0) and combinations thereof.7. (canceled)8. The process as claimed in claim 1 , wherein the reaction of step (ii) is carried out in presence of a solvent selected from toluene claim 1 , xylene claim 1 , N claim 1 ,N-dimethylformamide claim 1 , dimethylsufoxide claim 1 , tetrahydrofuran and 1 claim 1 ,4-dioxane or mixtures thereof claim 1 , and wherein the borylation reagent is selected from the group consisting of Bis(neopentylglycolato)diboron claim 1 , Bis(catecholato) ...

PROCESS FOR PREPARATION OF DAPAGLIFLOZIN

The present invention relates to a process for the preparation of amorphous dapagliflozin. The present invention relates to 2,3-butanediol solvate of dapagliflozin and process for its preparation. 4. The process of claim 1 , wherein in step (f) claim 1 , the alcohol is methanol and the ether is diisopropyl ether.5. The process of claim 1 , wherein in step (h) claim 1 , the alcohol is isopropyl alcohol and the hydrocarbon is cyclohexane.6. The process of claim 1 , wherein the step (i) of recovering dapagliflozin in amorphous form comprises:(i) removing the solvent from the solution obtained in step (h); or(ii) treating the solution of step (h) with an anti-solvent.7. The process of claim 6 , wherein the solvent is removed from the solution by concentrating the solution claim 6 , or completely evaporating the solvent claim 6 , or removing the solvent by one of lyophilisation claim 6 , freeze-drying claim 6 , spray drying claim 6 , fluid bed drying claim 6 , flash drying claim 6 , spin flash drying claim 6 , and thin-film drying.8. (canceled)10. The process of claim 9 , wherein the ether solvent is selected from the group consisting of diethyl ether claim 9 , diisopropyl ether claim 9 , methyl tert-butyl ether claim 9 , tetrahydrofuran claim 9 , and dioxane.11. The process of claim 9 , wherein the alcohol solvent is selected from the group consisting of methanol claim 9 , ethanol claim 9 , n-propyl alcohol claim 9 , and isopropyl alcohol.1224.-. (canceled) This application claims the benefit of Indian Provisional Applications 1790/MUM/2015 filed on May 5, 2015 and 201621002175 filed on Jan. 20, 2016, entitled “PROCESS FOR PREPARATION OF DAPAGLIFLOZIN”, the contents of which are incorporated herein by reference.The present invention relates to a process for the preparation of amorphous dapagliflozin. The present invention relates to 2,3-butanediol solvate of dapagliflozin and process for its preparation.Dapagliflozin, also known as D-glucitol, 1,5-anhydro-1-C-[4-chloro- ...

Solid form of (S)-[2-chloro-4-fluoro-5-(7-morpholin-4-yl-quinazolin-4-yl)phenyl]-(6-methoxy-pyridazin-3-yl)-methanol

An anhydrous disordered crystalline (S)-[2-chloro-4-fluoro-5-(7-morpholin-4-yl-quinazolin-4-yl)-phenyl]-(6-methoxy-pyridazin-3-yl)-methanol can be used in pharmaceutical compositions. 1: An anhydrous disordered crystalline (S)-[2-chloro-4-fluoro-5-(7-morpholin-4-yl-quinazolin-4-yl)-phenyl]-(6-methoxy-pyridazin-3-yl)-methanol.2: The anhydrous disordered crystalline (S)-[2-chloro-4-fluoro-5-(7-morpholin-4-yl-quinazolin-4-yl)-phenyl]-(6-methoxy-pyridazin-3-yl)-methanol according to claim 1 , which is characterized by a powder X-ray diffraction pattern having at least two peaks at degrees two theta selected from the group consisting of 3.9 claim 1 , 5.1 claim 1 , 6.1 claim 1 , 8.4 claim 1 , 10.7 claim 1 , 12.7 claim 1 , 14.6 claim 1 , and 22.8 claim 1 , each ±0.3 degrees two theta claim 1 , wherein each of the at least two peaks is characterized by having a full width at half maximum of equal to or greater than 0.2 degrees two theta.3: The anhydrous disordered crystalline (S)-[2-chloro-4-fluoro-5-(7-morpholin-4-yl-quinazolin-4-yl)-phenyl]-(6-methoxy-pyridazin-3-yl)-methanol according to claim 2 , wherein the powder X-ray diffraction pattern has at least one further peak at degrees two theta selected from 3.1 claim 2 , 9.9 claim 2 , 13.5 claim 2 , 16.0 claim 2 , 16.5 claim 2 , 18.0 claim 2 , 19.0 claim 2 , 20.9 claim 2 , 21.9 claim 2 , 22.8 claim 2 , 24.0 claim 2 , 24.9 claim 2 , and 25.4 each ±0.2 degrees two theta.4: The anhydrous disordered crystalline (S)-[2-chloro-4-fluoro-5-(7-morpholin-4-yl-quinazolin-4-yl)-phenyl]-(6-methoxy-pyridazin-3-yl)-methanol according to claim 1 , which is characterized by a powder X-ray diffraction pattern substantially in accordance with .5: The anhydrous disordered crystalline (S)-[2-chloro-4-fluoro-5-(7-morpholin-4-yl-quinazolin-4-yl)-phenyl]-(6-methoxy-pyridazin-3-yl)-methanol according to claim 1 , which is characterized by a differential scanning calorimeter profile substantially in accordance with .6: The anhydrous disordered ...

METHOD OF MANUFACTURING A PHARMACEUTICAL COMPOSITION

A method of manufacturing oxytocin or oxytocin receptor agonist comprising a step of combining an antisolvent with a solution comprising oxytocin or oxytocin receptor agonist so as to precipitate a product oxytocin or a product oxytocin receptor agonist from the solution. 131-. (canceled)32. A method of manufacturing oxytocin or oxytocin receptor agonist comprising:(i) performing liquid chromatography on a crude oxytocin or crude oxytocin receptor to obtain a liquid chromatography solution comprising oxytocin or oxytocin receptor agonist;(ii) performing solid-phase enrichment on the liquid chromatography solution obtained in step (i) to obtain a solid-phase enrichment solution comprising oxytocin or a oxytocin receptor agonist;(iii) distilling the solid-phase enrichment solution obtained in step (ii) to obtain dry solid oxytocin or dry solid oxytocin receptor agonist or a distillate solution of oxytocin or oxytocin receptor agonist having a reduced content of a solvent of the oxytocin or oxytocin receptor agonist relative to the solid-phase enrichment solution;(iv) if present following step (iii) redissolving the dry solid oxytocin or dry solid oxytocin receptor agonist to obtain a concentrated solution comprising oxytocin or oxytocin receptor agonist having a reduced content of a solvent of the oxytocin or oxytocin receptor agonist relative to the solid-phase enrichment solution; and(v) combining an antisolvent with the distillate of step (iii) or concentrated solution of step (iv) to precipitate a product oxytocin or a product oxytocin receptor agonist.33. A method according to claim 32 , wherein the crude oxytocin or crude oxytocin receptor agonist has a purity of less than 97%34. A method according to claim 32 , wherein the product oxytocin or product oxytocin receptor agonist has a purity greater than or equal to 97.5%.35. A method according to claim 32 , wherein a solvent in any solution comprising oxytocin or oxytocin receptor agonist is a polar solvent ...

METHOD FOR PREPARING IMIDAZOLE DERIVATIVE AND INTERMEDIATE THEREOF AND CRYSTAL FORM

Disclosed are a method for preparing an imidazole derivative and crystal form A and crystal form B thereof, and also disclosed is a method for preparing a compound of formula (I) and an intermediate thereof. 4. The process according to claim 2 , wherein the acid is selected from the group consisting of trifluoroacetic acid claim 2 , acetic acid claim 2 , hydrochloric acid claim 2 , dilute sulfuric acid and p-toluenesulfonic acid.6. The process according to claim 5 , wherein the insert solvent is a single solvent or a mixed solvent for several solvents selected from the group consisting of ethyl acetate claim 5 , isopropyl acetate claim 5 , methyl tent-butyl ether claim 5 , cyclohexane and n-heptane.7. The process according to claim 6 , wherein the insert solvent is a mixed solvent of ethyl acetate and n-heptane.10. Crystal form A or Crystal form B of the compound of formula (I) claim 6 , the XRPD spectrogram is shown in and claim 6 , respectively.11. A process for preparing crystal form A according to claim 10 , comprising adding the compound of formula (I) to an organic solvent claim 10 , heating to 30° C. to the reflux temperature to dissolve claim 10 , and then cooling to 0 to 20° C. within 0.5 to 10 hours to precipitate the crystal.12. The process for preparing crystal form A according to claim 11 , wherein the organic solvent is selected from the group consisting of dichloroethane claim 11 , a Calkyl alcohol claim 11 , a Cether or cyclic ether claim 11 , a Cketone claim 11 , a Cester claim 11 , benzene optionally substituted by methyl or ethyl or halogen atom(s) claim 11 , wherein the number of the substituent(s) is selected from 1 claim 11 , 2 and/or 3.13. The process for preparing crystal form A according to claim 12 , the organic solvent is selected from the group consisting of dichloromethane claim 12 , methanol claim 12 , ethanol claim 12 , isopropanol claim 12 , tetrahydrofuran claim 12 , dioxane claim 12 , 2-methyltetrahydrofuran claim 12 , acetone claim ...

Process for preparing bortezomib, intermediates, and crystalline forms thereof

The present disclosure provides a process for preparing Bortezomib, intermediates, and crystalline forms thereof.

METHOD FOR PRODUCING PARTICLES

The object of the disclosure is to provide a method for efficiently producing fine particles with low crystal growth of the raw material components, in particular fine particles with a plurality of raw material components in a highly complexed state and having low crystal growth, without blockage of the nozzle. The method of the disclosure for producing particles includes injecting a good solvent solution that includes a good solvent and one or more raw material components dissolved in the good solvent, with a nozzle into a precipitating poor solvent that has been heated to a temperature higher than the boiling point of the good solvent, to evaporate the good solvent solution and precipitate a plurality of particles, and running a cleansing poor solvent through the nozzle before starting and after completing injection of the good solvent solution into the precipitating poor solvent. 1. A method for producing particles , the method comprising:injecting a good solvent solution that comprises a good solvent and one or more raw material components dissolved in the good solvent, through a nozzle into a precipitating poor solvent that has been heated to a temperature higher than the boiling point of the good solvent, to evaporate the good solvent and precipitate a plurality of particles, andrunning a cleansing poor solvent through the nozzle before starting and after completing injection of the good solvent solution into the precipitating poor solvent.2. A method for producing particles according to claim 1 , further comprising running the good solvent solution and the cleansing poor solvent through the nozzle in an alternating manner.3. A method for producing particles according to claim 1 , further comprising mixing the good solvent solution and the cleansing poor solvent and running them through the nozzle.4. A method for producing particles according to claim 1 , wherein the cleansing poor solvent has a boiling point that is at or above the temperature of the ...

Continuous-Flow, Well Mixed, Microfluidic Crystallization Device for Screening Polymorphs, Morphologies and Crystallization Kinetics at Controlled Supersaturation

The disclosure relates to a microfluidic system for the screening of polymorphs, morphology, and crystallization kinetics under well-mixed, continuous-flow at controlled supersaturations. The disclosure also relates to a method for screening crystalline polymorphs and morphology, and crystallization kinetics. The microfluidic system includes a microfluidic chamber having one or more inlets, a passive mixing zone, and a trap zone. The passive mixing zone promotes mixing of solvent, solute, and optionally antisolvent under stable, controlled levels of supersaturation. The trap zone similarly has stable, controlled levels of supersaturation and correspondingly low velocity to retain solute crystals formed in the trap zone for time-dependent evaluation. 1. A microfluidic system comprising: (i) a first inlet zone in fluid communication with a first inlet adapted to receive a first fluid stream comprising a solute dissolved in a solvent,', '(ii) optionally a second inlet zone in fluid communication with a second inlet adapted to receive a second fluid stream,', '(iii) a passive mixing zone having (A) a first mixing zone boundary and (B) a second mixing zone boundary separate from the first mixing zone boundary, the passive mixing zone being in fluid communication with the first inlet zone via the first mixing zone boundary and, when present, the second inlet zone via the first mixing zone boundary,', '(iv) a trap zone having a trap zone boundary in fluid communication with the second mixing zone boundary, wherein the trap zone is positioned within the microfluidic chamber such that fluid flowing through the microfluidic chamber has a sufficiently low velocity to retain solute crystals formed in the trap zone within the trap zone,', '(v) an outlet zone in fluid communication (A) with the passive mixing zone via the first mixing zone boundary, and (B) an outlet adapted to discharge fluid from the microfluidic chamber, and', '(vi) optionally a first temperature control means ...

NOVEL INDUSTRIAL CRYSTALLIZATION METHOD OF CEFUROXIME SODIUM AND PREPARATION THEREOF

It discloses a new industrial crystallization method of Cefuroxime Sodium, wherein supercritical fluid extraction technology and traditional crystalline technology are combined to realize the recrystallization of Cefuroxime Sodium. Processes such as extraction, adsorption, crystallization and drying are carried out with a supercritical fluid, a solvent, an extraction cell and a crystallization tank to realize the recrystallization of Cefuroxime Sodium under a specific pressure at a specific temperature. 1. A novel industrial crystallization method of Cefuroxime Sodium , characterized in that , combining supercritical fluid extraction and traditional crystallization to realize the recrystallization of Cefuroxime Sodium , preferably dissolving Cefuroxime Sodium in an organic solvent , extracting the organic solvent and the solute in the solution of Cefuroxime Sodium by a supercritical fluid , and changing the solubility of the ingredients in the organic solvent and the supercritical fluid by adjusting the temperature and the pressure to make Cefuroxime Sodium crystallize.2. The method according to claim 1 , characterized in that including Cefuroxime Sodium prepared by the method claim 1 , and a sterile powder for injection containing Cefuroxime Sodium.3. The method according to claim 2 , characterized in that claim 2 , the solution of Cefuroxime Sodium is subjected to supercritical fluid extraction for 520 minutes under a pressure of 1540 MPa at a temperature of 4060° C. claim 2 , and Cefuroxime Sodium is crystallized and separated from its solution for 2040 minutes under a pressure of 0.55 MPa at a temperature of 2030° C.4. The method according to claim 3 , characterized in that claim 3 , said solvent for dissolving Cefuroxime Sodium is selected from one of alcohols claim 3 , aldehydes claim 3 , esters claim 3 , ketones claim 3 , ethers claim 3 , water and so on or a mixture thereof claim 3 , an aqueous ethanol is preferable claim 3 , and an aqueous ethanol with a ...

Processing post-industrial and post-consumer waste streams and preparation of post-industrial and post-consumer products therefrom

A system for and method of, processing post-consumer and post-industrial waste streams, producing active ingredients for waste stream processing, processing aqueous waste streams, preparing and collecting a multi-purpose chemical precursor, removing phosphates, nitrates, heavy metals, and other contaminants from aqueous waste streams, collecting and processing a post-consumer and post-industrial product from aqueous waste streams, administering and positioning assets and processes associated with waste stream processing, and scheduling operations for sub-systems of the system.

Method of preparing benzyl 4-amino-3-chloro-5-fluoro-6-(4-chloro-2-fluoro-3-methoxyphenyl)picolinate

A method of preparing benzyl 4-amino-3-chloro-5-fluoro-6-(4-chloro-2-fluoro-3-methoxyphenyl)picolinate (I) from benzyl 4,5-difluoro-6-(4-chloro-2-fluoro-3-methoxyphenyl)picolinate (II) is described. The method includes the use of amination and chlorination process steps to provide the compound of Formula I.

EUTECTIC EXTRACTION OF SOLIDS

The present in relates to methods and uses for preparing biological extracts using Deep Eutectic Solvents (DES) as hydrotropic agents, methods for purifying biological extracts formed using Deep Eutectic Solvents (DES) as hydrotropic agents, the biological extractions obtained using the methods and uses and the use of the biological extracts, such as in food-stuffs, flavours and fragrances, pharmaceuticals, cosmetics, nutraceuticals and supplements, such as food supplements and sports supplements. 1. A method for providing a solid biological extract comprising:i) mixing biological material with an extraction solution comprising water and a Deep Eutectic Solvent (DES);ii) removing any undissolved biological material from the solution obtained in (i);iii) obtaining a flocculate and/or precipitate by adding water to and/or cooling the solution obtained in step (ii);iv) collecting the resulting solid material obtained in step (iii) from the solution; andv) optionally drying the solid material obtained in step (iv).2. The method for providing the solid biological extract of :wherein the extraction solution of step i) is free of water.3. The method according to claim 1 , wherein the solid biological extract comprises at least 2% by weight of lipophilic claim 1 , hydrophobic claim 1 , oil soluble and/or non-water-soluble compounds.4. The method according to claim 3 , wherein the lipophilic claim 3 , hydrophobic claim 3 , oil soluble and/or non-water-soluble compounds comprise one or more of phenolic compounds including phenolic acids claim 3 , phenolic esters claim 3 , phenolic diterpenes claim 3 , flavonoids claim 3 , secoiridoids claim 3 , curcuminoids claim 3 , bixin claim 3 , capsaicinoids claim 3 , cannabinoids claim 3 , pyranoanthocyanins claim 3 , stilbenes claim 3 , phenolic alcohols claim 3 , phenolic lipids claim 3 , sylimarins claim 3 , alkaloids claim 3 , lipids claim 3 , phenylpropanoids claim 3 , coumarin claim 3 , organic acids claim 3 , terpenoids including ...

Pressure driven flow crystallizer

The present invention generally relates to systems and methods for pressure driven flow crystallization. In some embodiments, the system comprises a comprising a cavity and a mixing mechanism. In some embodiments, one or more inlets facilitate the transfer of one or more reagent streams to the cavity. In some such embodiments, the mixing mechanism mixes the first and second reagent streams such that a continuous crystallization and/or generation of a product (e.g., solid particles) in the fluid.

CRYSTALLISATION OF CHEMICAL MOLECULES

This invention relates to a method of forming crystals of chemical molecules. The methods are effective even when only very small amounts of a compound are available and can be used to explore the experimental crystallisation space including screening for optimal crystallisation conditions such as for polymorphic phases, salts, solvates and co-crystals of chemical molecules and to provide single crystals for structural determination of unknown molecules by single crystal X-ray crystallography. 1. A method forming a crystal of a chemical molecule or a salt thereof , the method comprising:a) forming a droplet, the droplet comprising a first liquid and a second liquid; wherein the first liquid comprises the chemical molecule or a salt thereof dissolved in an organic medium; and the second liquid is an oil; andb) allowing a crystal comprising the chemical molecule to form in the droplet.2. A method of claim 1 , wherein the chemical molecule is an organic molecule.3. A method of claim 1 , wherein the chemical molecule is a small molecule.4. A method of claim 1 , wherein the organic medium comprises at least one organic solvent.5. A method of wherein the total amount of organic solvent is greater than 75% by volume of the organic medium.6. A method of claim 1 , wherein at least one organic solvent in the organic medium has a boiling point greater than 80° C.7. A method of wherein at least one organic solvent in the organic medium has a boiling point greater than 125° C.8. A method of claim 1 , wherein the first liquid comprises less than 1 mg of the organic molecule claim 1 , or salt thereof.9. A method of claim 8 , wherein the first liquid comprises less than 100 μg of the organic molecule claim 8 , or salt thereof.10. A method of claim 1 , wherein the total volume of the first liquid in the droplet may be less than 1 μL.11. A method of claim 10 , wherein the total volume of the first liquid in the droplet may be less than 200 nL.12. A method of claim 1 , wherein the oil ...

CRYSTALLINE FORM A OF OBETICHOLIC ACID AND PREPARATION METHOD THEREOF

The present invention relates to crystalline Form A of obeticholic acid and the preparation method thereof. The present invention provides Form A having characteristic peaks at 2theta value of 4.9°±0.2°, 5.2°±0.2°, 9.9°±0.2°. The present invention provides a novel crystalline form of obeticholic acid, which has good stability, good processability and other favorable properties, and is suitable for storage and usage as a final product. In addition, the preparation method is simple, low cost, and has great value for the future optimization and development of obeticholic acid. 1. A crystalline Form A of Obeticholic acid , is characterized in that , the X-ray powder diffraction pattern of the crystalline Form A shows characteristic peaks at 2theta values of 4.9°±0.2° , 5.2°±0.2° , and 9.9°±0.2°.2. The crystalline Form A according to claim 1 , characterized in that claim 1 , the X-ray powder diffraction pattern of the crystalline Form A further shows characteristic peaks at 2theta values of 7.2°±0.2° claim 1 , 7.7°±0.2° claim 1 , and 10.5°±0.2°.3. The crystalline Form A according to claim 1 , characterized in that claim 1 , the X-ray powder diffraction pattern of the crystalline Form A further shows characteristic peaks at 2 theta values of 6.2°±0.2° claim 1 , 12.5°±0.2° claim 1 , and 15.7°±0.2°.4. The crystalline Form A according to claim 1 , characterized in that the X-ray diffraction pattern of the crystalline Form A is substantially the same as depicted in .5. The crystalline Form A according to claim 1 , characterized in that the differential scanning calorimetry analysis curve of said crystalline Form A shows an endothermic peak when heated to 90 ˜ 92° C.6. The crystalline Form A according to claim 1 , characterized in that said crystalline Form A is a hydrate.7. The crystalline Form A according to claim 1 , characterized in that claim 1 , the water content in said crystalline Form A is 4 wt %˜13 wt %.8. A process for preparing crystalline Form A of Obeticholic ...

TREATMENT OF PHOSPHATE-CONTAINING WASTEWATER AND METHODS FOR FINES CONTROL

Methods and apparatus for precipitating dissolved materials from an aqueous solution are provided. In an embodiment, the method comprises: introducing the aqueous solution into a reactor and introducing a source of magnesium (Mg) into the reactor in a quantity sufficient to cause the dissolved materials to precipitate into crystals. The source of Mg is introduced into the reactor in the form of particles of a Mg-containing material. The source of Mg has a solubility in the aqueous solution of less than about 1 g/L. Alternatively, the concentration of Mg in the reactor is less than about 0.03 mol/L. In an embodiment, the apparatus comprises a reaction tank having an inlet and an outlet and a hydration tank associated with the reaction tank and configured for hydrating a source of Mg in an aqueous solvent and introducing the source of Mg as a hydrated slurry into the reaction tank. 1. A method for precipitating dissolved materials from an aqueous solution , the method comprising:introducing the aqueous solution containing the dissolved materials into a reactor; andintroducing a source of magnesium (Mg) into the reactor in a quantity sufficient to cause the dissolved materials in the aqueous solution to precipitate into crystals, wherein the source of Mg is introduced into the reactor in the form of particles of a Mg-containing material, andwherein the source of Mg has a solubility in the aqueous solution of less than about 1 g/L and/or the concentration of available Mg in the reactor is less than about 0.03 mol/L.2. A method according to claim 1 , wherein the source of Mg is introduced as a hydrated slurry.3. A method according to claim 2 , further comprising making the hydrated slurry by adding water to the source of Mg and soaking the source of Mg for a hydration time before introducing the hydrated slurry into the reactor.4. (canceled)5. A method according to claim 1 , wherein the source of Mg has a solubility in aqueous solvent of about 5 mg/L to about 150 mg/L.6. ...

Recovering a caustic solution via calcium carbonate crystal aggregates

Techniques for converting a portion of a carbonate to hydroxide include receiving an alkaline carbonate solution that includes between 0.1M (moles per liter of solution) to 4.0M hydroxide and between 0.1M to 4.1M carbonate; reacting, in a slaking process, quicklime (CaO) and a low carbonate content fluid to yield a slurry of primarily slaked lime (Ca(OH) 2 ); and reacting the Ca(OH) 2 slurry and the alkaline carbonate solution to grow calcium carbonate (CaCO 3 ) crystal aggregates of 0.0005 mm 3 to 5 mm 3 in volume in a fluidized-bed reactive crystallizer.

Crystalline form of fused pyridine derivative's maleate and uses thereof

The compound of Formula I, the crystalline form thereof, and methods of preparing and using them are provided.

Method for Extracting Lithium from Salt Lake Brine and Simultaneously Preparing Aluminum Hydroxide

The present disclosure relates to a method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide. This method includes: a. adding an aluminum salt to the brine to obtain a mixed salt solution A, adding an alkali solution to the mixed salt solution A for co-precipitation reaction, then subjecting to crystallization reaction and solid-liquid separation at the end of the reaction to obtain magnesium-aluminum hydrotalcite solid product and lithium-containing brine, wherein in step a, the alkali solution is an alkali solution free of carbonate ion; b. evaporating and concentrating the lithium-containing brine to obtain a lithium-rich brine, adding an aluminum salt to the lithium-rich brine to obtain a mixed salt solution B, adding an alkali solution dropwise to the mixed salt solution B to perform a co-precipitation reaction and solid-liquid separation after the end of the reaction to obtain a lithium-containing liquid and a lithium-containing layered material filter cake, wherein in step b, the alkali solution is an alkali solution free of carbonate ion; c. dispersing the lithium-containing layered material filter cake in deionized water to form a suspension slurry, then adjusting the pH value of the suspension slurry so as to carry out a lithium deintercalation reaction; d. filtering the slurry obtained after the lithium deintercalation reaction to obtain a lithium-containing solution and aluminum hydroxide filter cake; e. washing the aluminum hydroxide filter cake with deionized water and drying to obtain aluminum hydroxide solid.

PLINABULIN COMPOSITIONS

Disclosed herein are plinabulin polymorphs, compositions, their use and preparation as therapeutic agents. In particular, some embodiments relate to plinabulin monohydrate in a crystalline form. 1. A plinabulin monohydrate in crystalline form , exhibiting an X-ray powder diffraction pattern comprising at least three characteristic peaks selected from the group consisting of peaks at approximately 8.1° , 13.1° , 16.3° , 23.9° , 24.2° , 24.5° , and 26.6° 2θ.2. The plinabulin monohydrate of claim 1 , exhibiting an X-ray powder diffraction pattern comprising at least peaks at approximately 8.1° claim 1 , 13.1° claim 1 , 16.3° claim 1 , 23.9° claim 1 , 24.2° claim 1 , 24.5° claim 1 , and 26.6° 2θ.3. The plinabulin monohydrate of claim 1 , exhibiting an X-ray powder diffraction pattern comprising at least peaks at approximately 8.1° claim 1 , 13.1° claim 1 , 16.1° claim 1 , 16.3° claim 1 , 19.8° claim 1 , 22.9° claim 1 , 23.9° claim 1 , 24.2° claim 1 , 24.5° claim 1 , 26.6° claim 1 , and 29.3° 2θ.4. The plinabulin monohydrate of claim 1 , wherein the crystalline form has a melting point of about 267° C.5. The plinabulin monohydrate of claim 1 , having a differential scanning calorimetry thermogram with endothermic peaks at about 141° C. and about 267° C.6. A plinabulin composition claim 1 , comprising more than about 50% by weight of the plinabulin monohydrate of claim 1 , based on the total weight of the composition.7. The composition of claim 6 , comprising more than about 75% by weight of the plinabulin monohydrate claim 6 , based on the total weight of the composition.8. (canceled)9. The composition of claim 6 , comprising more than about 95% by weight of the plinabulin monohydrate claim 6 , based on the total weight of the composition.10. (canceled)11. The composition of claim 6 , comprising more than about 99% by weight of the plinabulin monohydrate claim 6 , based on the total weight of the composition.12. (canceled)13. (canceled)14. (canceled)15. A plinabulin ...

POLYMER PARTICLE, MANUFACTURING METHOD THEREOF, AND SEPARATOR FOR BATTERY COMPRISING THE SAME

The present application relates to a polymer particle manufacturing method, and according to an example of the manufacturing method and a manufacturing apparatus therefor, a reduction in energy can be achieved by simplifying a manufacturing process thereof. 1. A polymer particle manufacturing method , comprising mixing a second solvent with a first polymer solution which is at or above (T+5)° C. and includes a polymer dissolved in a first solvent (where Tis a melting point (unit: ° C.) of the polymer).2. The polymer particle manufacturing method of claim 1 , wherein a mixture solution of the first polymer solution and the second solvent is a non-emulsion.3. The polymer particle manufacturing method of claim 1 , wherein the first solvent is a good solvent with respect to the polymer.4. The polymer particle manufacturing method of claim 1 , wherein the first solvent has a Hansen relative energy difference of 0.6 or more and less than 2 claim 1 , with respect to the polymer at room temperature.5. The polymer particle manufacturing method of claim 1 , wherein the second solvent has a Hansen relative energy difference of more than 2 and less than 5 with respect to the polymer at room temperature.6. The polymer particle manufacturing method of claim 1 , wherein the polymer is a polyolefin.7. The polymer particle manufacturing method of claim 1 , wherein the first solvent is a monovalent alcohol and the second solvent is a monovalent alcohol or ketone.8. The polymer particle manufacturing method of claim 1 , wherein the first solvent is a monovalent alcohol having 6 or more carbons.9. The polymer particle manufacturing method of claim 1 , wherein the second solvent is a monovalent alcohol having 5 or less carbons claim 1 , or ketone.10. The polymer particle manufacturing method of claim 1 , wherein a temperature of the second solvent to be mixed with the first polymer solution is adjusted to a range of (T−70)° C. to T° C. (where Tis a boiling point (unit: ° C.) of the ...

Method for producing microparticles from pressurized and heated starting material solution

The present invention addresses the problem of providing a method for efficiently producing uniform microparticles of curcumin and/or γ-oryzanol at a higher yield. The target microparticles are produced by dissolving a starting material in a solvent to give a starting material solution and then subjecting the starting material solution to crystallization by a poor solvent method to thereby deposit the starting material. To prepare the starting material solution, curcumin and/or γ-oryzanol are used as the starting material(s) and ethanol is used as the solvent. The starting material(s) and the solvent are stirred in a pressurized state at a temperature of 78.3-130° C. inclusive to give the starting material solution. Then, the starting material solution thus obtained is subjected to crystallization by the poor solvent method and thus the target microparticles are produced.

Method for improving nucleation of crystals from solution

The present invention is related to a method for nucleating crystals from a solution comprising the steps of: injecting in a first capillary () tube an under saturated solution comprising a solvent and a soluble compound to be crystallised; changing the local conditions of the solution downstream of the capillary tube () to supersaturated conditions above the metastable conditions, the transition time of the fluid flowing in the capillary tube between the under saturated conditions and the supersaturated conditions above the metastable conditions being less than 1000 ms, preferably below 100 ms, even more preferably less than 10 ms. 1. A method for nucleating crystals from a solution comprising the steps of:injecting in a first capillary tube an undersaturated solution comprising a solvent and a soluble compound to be crystallised; andchanging the local conditions of the solution downstream of the first capillary tube to supersaturated conditions above the metastable conditions, wherein a transition time of a fluid flowing in the first capillary tube between the undersaturated conditions and the supersaturated conditions above the metastable conditions is less than 1000 ms.2. The method according to wherein a supersaturation difference between the undersaturated solution and the supersaturated solution is at least 1 claim 1 , supersaturation being defined as the relative difference between a local concentration of the compound to be crystallised and the solubility of a compound to be crystallised.3. The method according to wherein a transition to supersaturated conditions is obtained by at least one of the steps of:cooling down a capillary wall to a temperature below a metastable temperature,injecting an antisolvent into the injected undersaturated solution, andinjecting a cooled solvent into the injected undersaturated solution,the one or more of the cooled solvent or antisolvent being injected by a second capillary tube having essentially the same dimension as the ...

PROCESS FOR THE PREPARATION OF ISOCARBOXAZID

This invention relates to a novel chemical process for the synthesis of N′-benzyl-5-methylisoxazole-3-carbohydrazide (Isocarboxazid) which comprises reacting 5-methyl-3-isoxazole carboxylic acid ester with benzylhydrazine or a salt thereof in an aprotic organic solvent and in the presence of an organic base. 2. The process according to claim 1 , further comprisingb) isolating the material as Isocaboxazid (I) and optionallyc) re-crystallizing the isolated Isocaboxazid (I) obtained in step (b).3. The process according to claim 1 , wherein R in formula (II) is methyl.4. The process according to claim 1 , wherein the aprotic solvent is toluene claim 1 , heptane claim 1 , cyclohexane claim 1 , isopropyl acetate or a mixture thereof.5. The process according to claim 1 , wherein the organic base is triethylamine.6. The process according to claim 1 , wherein the reaction is performed at a temperature below 50°.7. The process according to claim 6 , wherein the temperature is in the range of 25° C. to 50° C.8. The process according to claim 1 , wherein the compound (III) is benzylhydrazine dihydrochloride.9. The process according to claim 2 , wherein the re-crystallization is performed by dissolving the product obtained in step (b) in a solvent selected from acetone claim 2 , methanol claim 2 , acetic acid and DMSO claim 2 , or a mixture thereof at a temperature between 20 and 40° C. claim 2 , followed by the addition of an anti-solvent selected from water claim 2 , toluene claim 2 , alkanes claim 2 , and cycloalkanes claim 2 , or a mixture thereof claim 2 , or a mixture of water and isopropanol.10. The process according to claim 1 , wherein the amount of said aprotic solvent is in the range of 8 to 15 Volumes.11. The process according to claim 1 , wherein the ratio between said organic base and benzylhydrazine (III) is in the range of 1.9 to 2.2 mol/mol.12. The process according to claim 5 , wherein the ratio between triethylamine and benzylhydrazine (III) is in the range of ...

Equipment Assembly for and Method of Processing Particles

An equipment assembly for preparing, harvesting and collecting particles is disclosed. The assembly comprises a tandem filter system with one or more high pressure filters, one or more low pressure filters and one or more collection vessel. Particles can be prepared, harvested and collected continuously, semi-continuously or in a batch-type operation. A tandem filter system and its method of use are also disclosed. Particles made with the assembly and according the instant methods are also disclosed. The assembly provides improved particle harvesting and collection over other systems and permits continuous particle formation, in particular by dispersion of a solute-containing process fluid within a supercritical anti-solvent. 138.-. (canceled)39) A particle formation and collection equipment assembly comprising:at least one high pressure particle formation system that forms a supercritical fluid particle-containing suspension;downstream of and conductively engaged with the at least one high pressure particle formation system, at least one first valve; downstream of and conductively engaged with the at least one first valve, at least one second valve;', 'downstream of and conductively engaged with the at least one second valve, at least one high pressure harvesting filter system;', 'downstream of and conductively engaged with the at least one second valve, at least one collection vessel system; and', 'downstream of and conductively engaged with the at least one collection vessel system, at least one low pressure collection filter system., 'downstream of and conductively engaged with the at least one first valve, at least two particle collection systems in parallel, wherein each of the at least two particle collection systems comprises40) The particle formation and collection equipment assembly of claim 39 , wherein the at least one first valve is adapted to direct the supercritical fluid particle-containing suspension alternately or sequentially to the at least two ...

CRYSTAL FORM A OF 1-ISOBUTYRYL-1'-((1-(4,4,4-TRIFLUOROBUTYL)-4,5,6,7-TETRAHYDRO-1H-BENZO[D]IMIDAZOL-2-YL)METHYL)SPIRO[AZETIDINE-3,3'-INDOLIN]-2'-ONE

Disclosed are a method for preparing an imidazole derivative and crystal form A and crystal form B thereof, and also disclosed is a method for preparing a compound of formula (I) and an intermediate thereof. 3. A process for preparing the crystal form B according to claim 1 , wherein the process comprises the following steps:{'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, '(1) admixing the compound of formula (I) according to with a polar organic solvent to form a mixture, and'}(2) then slowly dropping water to the mixture formed in step (1) to precipitate the crystal.4. The process according to claim 3 , wherein the polar organic solvent is selected from the group consisting of a Calkyl alcohol claim 3 , a Calkyl ether or a Ccyclic ether and a Cketone.5. The process according to claim 4 , wherein the polar organic solvent is selected from the group consisting of methanol claim 4 , ethanol claim 4 , isopropanol claim 4 , tetrahydrofuran claim 4 , 2-methyltetrahydrofuran claim 4 , dioxane and acetone.6. A method for inhibiting respiratory syncytial virus activity in a subject claim 1 , comprising administering to the subject in need thereof a therapeutically effective amount of the crystal form B according to .7. The method according to claim 6 , wherein the subject has respiratory virus infection.8. A pharmaceutical composition comprising a therapeutically effective amount of the crystal form B according to as an active ingredient and a pharmaceutically acceptable carrier.9. A method for inhibiting respiratory syncytial virus activity in a subject claim 8 , comprising administering to the subject in need thereof a therapeutically effective amount of the pharmaceutical composition according to .10. The method according to claim 9 , wherein the subject has respiratory virus infection. The present application is a Divisional of U.S. application Ser. No. 15/580,167, filed Dec. 6, 2017, which is a 371 National Stage application of PCT/CN2016/085104, filed Jun. 7, 2016, ...

PROCESS FOR PREPARING 1-ISOBUTYRYL-1'-((1-(4,4,4-TRIFLUORO-BUTYL)-4,5,6,7- TETRAHYDRO-1H-BENZO[D]IMIDAZOL-2-YL)METHYL)SPIRO[AZETIDINE-3,3'-INDOLIN]-2'-ONE

Disclosed are a method for preparing an imidazole derivative and crystal form A and crystal form B thereof, and also disclosed is a method for preparing a compound of formula (I) and an intermediate thereof. 4. The process according to claim 2 , wherein the acid is selected from the group consisting of trifluoroacetic acid claim 2 , acetic acid claim 2 , hydrochloric acid claim 2 , dilute sulfuric acid and p-toluenesulfonic acid.7. The process according to claim 5 , wherein the insert solvent is a single solvent or a mixed solvent for several solvents selected from the group consisting of ethyl acetate claim 5 , isopropyl acetate claim 5 , methyl tert-butyl ether claim 5 , cyclohexane and n-heptane.8. The process according to claim 7 , wherein the insert solvent is a mixed solvent of ethyl acetate and n-heptane. The present application is a Continuation of U.S. application Ser. No. 16/242,753, filed Jan. 8, 2019, which is a Divisional of U.S. application Ser. No. 15/580,167, filed Dec. 6, 2017, which is a 371 National Stage application of PCT/CN2016/085104, filed Jun. 7, 2016, which claims priority from Chinese Application No. 201510309106.4, filed Jun. 8, 2015, the entire contents of which is hereby incorporated by reference.The present invention relates to a method for preparing an imidazole derivative, crystal form A, crystal form B, and the corresponding preparation process thereof, the present invention also relates to a method for preparing an intermediate of the compound of formula (I).Respiratory syncytial virus (RSV) is the main cause of severe lower respiratory tract infection in infants, children, the elderly and those with impaired immunity. Severe viral infections can cause bronchiolitis or pneumonia that require hospitalization or cause death (JAMA, 1997, 277, 12). Recently, Ribavirin has been approved for the treatment of the virus infection. Ribavirin is a nucleoside analog that is administered intranasally in the form of an aerosol. And the toxicity ...

METHODS FOR THE ISOLATION OF EXTRACELLULAR VESICLES AND OTHER BIOPARTICLES FROM URINE AND OTHER BIOFLUIDS

Compositions and methods for the isolation of protein-nucleic acid complexes and microvesicles (collectively referred to as “bioparticles”) released by mammalian cells into body fluids or cell culture media are provided. Isolated bioparticles of the invention contain biological molecules that are useful as diagnostic/prognostic biomarkers or for identification of therapeutic targets (e.g., disease or disorder-associated miRNAs). The isolation of biological molecules as described herein results in purification and concentration of the molecules. Methods for producing bio fluids that are free of detectable bioparticles, that are largely depleted of bioparticles, or that possess a reduced concentration of bioparticles compared to a bio fluid starting material (collectively termed “bioparticle-depleted”) are also provided. Isolation of bioparticle-depleted biofluid is useful, e.g., in experimental systems where it is desirable to use a biofluid that does not contain endogenous bioparticles, or has been substantially depleted of endogenous bioparticles, from the source material. 1. A method for isolating bioparticles from a liquid sample comprising:a) obtaining a liquid sample from a subject or cell culture;b) contacting said liquid sample with a crystal/precipitation-inducing agent under conditions suitable to allow for crystal formation and/or precipitation, thereby creating an admixture;c) incubating said admixture for a period of time sufficient to allow for crystal formation and/or precipitation; andd) separating said admixture to obtain a particle fraction containing bioparticles, thereby isolating bioparticles from said liquid sample.2. The method of claim 1 , wherein:the crystal/precipitation-inducing agent is selected from the group consisting of monosodium urate, uric acid, a salt thereof and a combination thereof;said admixture is present in an array of admixtures, optionally said array is a 96 well array;said admixture volume is less than about 1 ml;said step ...

Solution blending process for the fabrication of nylon6-montmorillonite nanocomposites

In general the present disclosure relates to Nylon 6/montmorillonite clay nanocomposites with enhanced mechanical properties that have been prepared primarily by solution compounding. A major challenge in producing the Nylon 6/montmorillonite clay nanocomposites is associated with the exfoliation and dispersion of the clay particles within the polymer matrix. This disclosure presents compositions and methods for obtaining highly or fully exfoliated nylon 6/montmorillonite nanocomposites not only for organically modified clays with known compatibility with nylon 6 (Cloisite 30B), but also for clays with low/no compatibility with nylon 6 (Cloisite 15A and Na—MMT) through solution compounding.

PREPARATION METHODS FOR PALBOCICLIB FREE BASE CRYSTAL FORM A AND CRYSTAL FORM B

Disclosed is a preparation method for a Palbociclib free base crystal form A as shown in Formula I, comprising the following steps: treating a Palbociclib free base and/or a Palbociclib salt compound by using an inorganic base in a water solvent at the temperature of 35 to 100′C. to obtain a Palbociclib free base crystal form A, the water solvent being water or mixed solvent obtained by water and an organic solvent capable of being mixed and disclosed in the water. Also disclosed is a preparation method for a Palbociclib free base crystal form B, comprising the following steps: treating a Palbociclib salt compound by using an inorganic base in a water solvent at the temperature of 0 to 20° C. to obtain a Palbociclib free crystal form B, the water solvent being water or a mixed solvent obtained by water and an organic solvent capable of being mixed and dissolved in the water. The method is safe and convenient in operation and low in pollution, and facilitates industrial production. 2. The method according to claim 1 , wherein the pharmaceutically acceptable salt of palbociclib is selected from the group consisting of palbociclib isethionate claim 1 , palbocklib hydrochloride claim 1 , palbociclib sulfate claim 1 , and palbociclib methane sulfonate or a combination thereof.3. The method according to claim 1 , wherein the volume ratio of water and the water-miscible organic solvent in the aqueous solvent is 1:0 to 1:20.4. The method according to claim 1 , wherein the water-miscible organic solvent is selected from the group consisting of methanol claim 1 , ethanol and isopropanol.5. The method according to claim 1 , wherein the inorganic base is selected from the group consisting of sodium hydroxide claim 1 , potassium hydroxide claim 1 , sodium carbonate and potassium carbonate.6. The method according to claim 1 , wherein the volume ratio of water and the water-miscible organic solvent in the aqueous solvent is 1:0 to 1:2.7. The method according to claim 1 , wherein ...

PLINABULIN COMPOSITIONS

Disclosed herein are plinabulin polymorphs, compositions, their use and preparation as therapeutic agents. In particular, some embodiments relate to plinabulin monohydrate in a crystalline form. 153-. (canceled)54. A plinabulin composition , comprising plinabulin and no more than about 10% by weight of impurities , based on the total weight of the composition.55. The plinabulin composition of claim 54 , wherein the plinabulin comprises no more than about 5% by weight impurities claim 54 , based on the total weight of the composition.56. The plinabulin composition of claim 55 , wherein the plinabulin comprises no more than about 1.9% by weight impurities claim 55 , based on the total weight of the composition57. The plinabulin composition of claim 54 , wherein the no more than about 10% by weight of impurities is based on the total weight of the composition other than water.58. The plinabulin composition of claim 54 , wherein the impurities includes one or more impurities introduced during the synthesis of plinabulin.59. The plinabulin composition of claim 58 , wherein the impurities can include dimethylformamide claim 58 , ethanol claim 58 , ethyl acetate claim 58 , methanol claim 58 , toluene claim 58 , acetic acid claim 58 , and residual solvent.60. The plinabulin composition of claim 54 , wherein the plinabulin composition includes no more than about 5% by weight of impurities claim 54 , based on the total weight of the composition other than water.61. The plinabulin composition of claim 60 , wherein the plinabulin composition includes no more than about 1.9% by weight of impurities claim 60 , based on the total weight of the composition other than water.62. The plinabulin composition of claim 54 , wherein the plinabulin composition comprises plinabulin and no more than about 5% by weight of impurities other than solvent molecules claim 54 , based on the total weight of non-solvent molecules in the composition.63. The plinabulin composition of claim 62 , wherein ...

COMPOSITIONS OF PARTICULATE COFORMULATION

Embodiments of the invention provide a composition of a particulate coformulation which includes particles containing an active substance and an additive, wherein each particle contains a relative additive concentration increasing radially outwards from a particle center to a particle surface along a finite gradient. In one example, the particle surface is an additive-rich surface without a distinct physical boundary between the particle center and the particle surface. The relative additive concentration may have a continuous rate of change across the finite gradient. In some examples, an active substance:additive ratio of the particle surface is sufficiently low to form a protective surface layer around the active substance. Generally, the particle surface is free of the active substance. 1. A method of preparing a particulate co-formulation , the method comprising:(i) dissolving an active substance and an additive in a vehicle to form a single phase target solution;(ii) co-introducing into a particle formation vessel, (a) a supercritical fluid that is miscible in all proportions with the vehicle and in which the active substance and the additive are insoluble or substantially insoluble, and (b) the target solution, such that the supercritical fluid and target solution enter the vessel at the same point and under conditions effective to disperse the target solution in the supercritical fluid and extract the vehicle therefrom, to thereby form a co-precipitated particulate product that is a solid dispersion of the active substance and the additive,wherein the particles of the particulate product have a finite gradient in relative additive concentration that increases radially outwards from the core to the surface of the particles, such that the particles comprise an additive-rich surface region but do not possess separate core and coating layers with a distinct physical boundary between them.2. The method of claim 1 , wherein the active substance is selected from ...

Divalent Ion Removal From Monoethylene Glycol-Water Streams

A system and process for the removal of divalent ions from a MEG-water stream are presented. The system includes a chemical treatment tank that receives the MEG-water stream, means for precipitating the calcium, magnesium, and hydroxide ions that are contained in the MEG-water stream, means for discharging the MEG-water stream from the chemical treatment tank, and means for recycling the discharged MEG-water stream back to the chemical treatment tank or routing it to a solids removal system. The means for precipitating the calcium, magnesium, and sulfate ions may be employed simultaneously or sequentially. 120-. (canceled)21. A process comprising:routing a monoethylene glycol (MEG) water stream containing sulfate ions to a vessel;adding barium chloride to the MEG-water stream; andforming and precipitating barium sulfate in the MEG-water stream to form a treated MEG-water stream.22. The process of claim 21 , further comprising adding a solution of sodium carbonate claim 21 , a solution of sodium hydroxide claim 21 , or both to the MEG-water stream to precipitate calcium claim 21 , magnesium or both.23. The process of claim 21 , further comprising discharging the treated MEG-water stream from the vessel claim 21 , recycling a first portion of the treated MEG-water stream to the vessel claim 21 , and routing a second portion of the treated MEG-water stream to a solids removal system.24. The process of claim 21 , further comprising routing the treated MEG-water stream to a solids removal system claim 21 , separating barium sulfate solids in the solids removal system claim 21 , and recycling the treated MEG-water stream to the vessel after it passes through the solids removal system.25. The process of claim 21 , further comprising routing the treated MEG-water stream to a solids removal system and then to a filtrate tank.26. The process of claim 22 , wherein the solution of sodium carbonate claim 22 , the solution of sodium hydroxide claim 22 , or both claim 22 , and the ...

PROCESS AND APPARATUS FOR PRECIPITATION OF POLY(PHENYLENE ETHER)

A process and system for the precipitation of poly(phenylene ether) is described. Precipitated poly(phenylene ether) obtained by the processes disclosed herein are in the form of poly(phenylene ether) particles having a bulk density of 150 to 500 kg/m, preferably 250 to 500 kg/m. 1. A process for precipitating polyphenylene ether , the process comprisingintroducing an anti-solvent to a mechanically stirred vessel containing a polyphenylene ether solution comprising a polyphenylene ether and a solvent to provide a mixture;{'sup': '3', 'agitating the mixture under conditions effective to provide precipitated polyphenylene ether particles having a bulk density of 150 to 500 kg/m; and recovering the precipitated polyphenylene ether particles.'}2. The process of claim 1 , wherein the anti-solvent comprises methanol claim 1 , ethanol claim 1 , isopropanol claim 1 , n-butanol claim 1 , acetone claim 1 , methyl ethyl ketone claim 1 , or a combination comprising at least one of the foregoing.3. A process for precipitating polyphenylene ether claim 1 , the process comprisingintroducing an anti-solvent to a mechanically stirred vessel comprising a polyphenylene ether solution comprising a polyphenylene ether and a solvent to provide a mixture comprising a precipitated polyphenylene ether; adding a first amount of the anti-solvent effective to provide a volume ratio of solvent to anti-solvent of 60:40 to 80:20, and agitating the slurry for 10 to 90 minutes;', 'adding a second amount of the anti-solvent effective to provide a volume ratio of solvent to anti-solvent of 35:65 to 55:45, and agitating the slurry for 10 to 90 minutes; and', 'adding a third amount of the anti-solvent effective to provide a volume ratio of solvent to anti-solvent of 10:90 to 30:70, and agitating the slurry for 30 to 90 minutes; and, 'wherein introducing the anti-solvent comprises'}{'sup': '3', 'recovering precipitated polyphenylene ether particles having a bulk density of 150 to 500 kg/m.'}4. The ...

PREPARATION METHODS FOR PALBOCICLIB FREE BASE CRYSTAL FORM A AND CRYSTAL FORM B

Disclosed is a preparation method for a Palbociclib free base crystal form A as shown in Formula I, comprising the following steps: treating a Palbociclib free base and/or a Palbociclib salt compound by using an inorganic base in a water solvent at the temperature of 35 to 100° C. to obtain a Palbociclib free base crystal form A, the water solvent being water or mixed solvent obtained by water and an organic solvent capable of being mixed and disclosed in the water. Also disclosed is a preparation method for a Palbociclib free base crystal form B, comprising the following steps: treating a Palbociclib salt compound by using an inorganic base in a water solvent at the temperature of 0 to 20° C. to obtain a Palbociclib free crystal form B, the water solvent being water or a mixed solvent obtained by water and an organic solvent capable of being mixed and dissolved in the water. The method is safe and convenient in operation and low in pollution, and facilitates industrial production. 2. The method according to claim 1 , the method comprising the following steps:1) treating a palbociclib free base with an inorganic base in an aqueous solvent at a temperature of 35° C. to 100° C. to obtain a crystal form A of palbociclib free base; or2) dissolving a palbociclib salt compound and optionally palbociclib free base in an aqueous solvent to form a solution, then treating the solution with an inorganic base water solution at a temperature of 35° C. to 100° C. to obtain a crystal form A palbociclib free base;wherein the aqueous solvent is water or a mixed solvent of water and water-miscible organic solvent.3. The method according to claim 1 , characterized in that the palbociclib salt compound is selected from the group consisting of palbociclib isethionate claim 1 , palbociclib hydrochloride claim 1 , palbociclib sulfate claim 1 , and palbociclib methane sulfonate or a combination thereof.4. The method according to claim 1 , characterized in that the palbociclib free base is ...

Cannabis-based therapeutic product for treatment of chronic pain

A cannabis-based therapeutic product for treatment of chronic pain produced by separating hash resin from plant material of the cannabis plant, pressing the hash resin to expel oil, leaving spent hash resin, extracting further cannabinoids from the spent hash resin using MCT oil, separating the cannabis compounds from the oils using high pressure liquid chromatography, flash chromatography, or similar techniques, and processing selected cannabis compound formulations into a form suitable for administration as a therapeutic product for treatment of chronic pain. The therapeutic product has at least 28% w/w cannabinol (CBD), and at least 2% w/w β-myrcene.

CRYSTALLINE FORM OF CANAGLIFLOZIN AND A METHOD OF ITS PREPARATION

The invention relates to a new crystalline form of Canagliflozin of formula I, with its systematic name (2S,3R,4R,5S,6R)-2-(3-((5-(4-fluorophenyl)thiophen-2-yl) methyl)-4-methylphenyl)-6-(hydroxymethyl)tetrahydro-2H-pyran-3,4,5-triol5 and a method of its preparation. 2. The canagliflozin of form X-C in accordance with claim 1 , further comprising the following characteristic reflections: 4.0; 16.2; 19.5 and 20.2 ±0.2° 2-theta.3. A method for preparing the crystalline form X-C of Canagliflozin defined in claim 1 , comprising the steps of:dissolving crystalline or amorphous Canagliflozin under boiling in a suitable etheric solvent selected from the group consisting of cyclopentyl methyl ether, t-butyl methyl ether and 2-methyltetrahydrofuran; drying the obtained solution by means of azeotropic distillation; cooling and/or adding an antisolvent in hot state wherein the antisolvent is selected from the group consisting of heptane, cyclohexane and hexane and then cooling the solution; and isolating the crystallized product.4. The method for preparing in accordance with claim 3 , wherein the procedure is carried out under an inert atmosphere of nitrogen or argon.5. The method for preparing in accordance with claim 3 , wherein the etheric solvent is cyclopentyl methyl ether and the antisolvent is heptane.6. The method for preparing in accordance with claim 3 , wherein the etheric solvent is 2-methyltetrahydrofuran and the antisolvent is heptane.7. The method for preparing in accordance with claim 5 , wherein the obtained solution is cooled down to a temperature in the range of 70-90° C. before the step of adding of the antisolvent.8. The method for preparing in accordance with claim 3 , wherein the etheric solvent is t-butyl methyl ether optionally with t-butanol.9. The method for preparing in accordance with claim 8 , wherein the obtained solution is cooled down to a temperature in the range of 50-60° C. before adding the antisolvent.10. The method for preparing in ...

Cannabis farming systems and methods

Variable-scale, modular, easily manufacturable, energy efficient, reliable, and computer-operated farming superstructure systems (FSS) may be used to produce cannabis for human consumption with minimal water and environmental impact. A system for producing electricity, heat, and cannabis includes a power production system (PPS), a farming superstructure system (FSS), and a temperature control unit (TCU). Methods to method to separate volatiles from cannabis are described. Methods to asexually clone a plurality of cannabis plants are also provided. Cannabinoid product processing systems are described (emulsion mixing system, evaporation system, spray drying system, crystallization, foodstuff preparation system, softgel encapsulation system).

METHOD FOR PREPARING ANTI-HEART-FAILURE MEDICINE LCZ696

The present invention discloses a method for preparing an anti-heart-failure medicine LCZ696. The preparing method comprises the following step (formula (I)): in an organic solvent, a Sacubitril dicyclohexylamine salt reacts with valsartan under the effect of a sodium hydroxide aqueous solution, and the anti-heart-failure medicine LCZ696 is obtained. The preparing method of the present invention is simple in process and omits the procedures of ion exchange from a sodium salt to a calcium salt and hydrochloric acid dissociation in an existing production process, residues of calcium ions are avoided, and the production efficiency is effectively improved. 2. The preparing method according to claim 1 , wherein the organic solvent is a mixed solvent of isopropyl acetate and acetone claim 1 , a mixed solvent of isopropyl acetate and acetonitrile claim 1 , or acetonitrile; andthe preparing method comprises the following steps: dissolving the Sacubitril dicyclohexylamine salt in the organic solvent, adding the valsartan after the obtained solution is clear by raising temperature, then adding the sodium hydroxide aqueous solution dropwise, and performing crystallization.3. The preparing method according to claim 1 , wherein the molar ratio of the Sacubitril dicyclohexylamine salt to the valsartan is 1:0.95-1.10 claim 1 , and preferably 1:1.05; and/orthe molar ratio of the Sacubitril dicyclohexylamine salt to sodium hydroxide is 1:2.95-3.10, and preferably 1:3.05; and/orthe mass percent concentration of the sodium hydroxide aqueous solution is 30%-40%.4. The preparing method according to claim 2 , wherein after the sodium hydroxide aqueous solution is added dropwise and before performing crystallization claim 2 , when the organic solvent is the mixed solvent of isopropyl acetate and acetone or the mixed solvent of isopropyl acetate and acetonitrile claim 2 , operation step (i) is performed: adding the isopropyl acetate dropwise and performing reducing pressure distillation ...

Equipment Assembly for and Method of Processing Particles

An equipment assembly for preparing, harvesting and collecting particles is disclosed. The assembly comprises a tandem filter system with one or more high pressure filters, one or more low pressure filters and one or more collection vessel. Particles can be prepared, harvested and collected continuously, semi-continuously or in a batch-type operation. A tandem filter system and its method of use are also disclosed. Particles made with the assembly and according the instant methods are also disclosed. The assembly provides improved particle harvesting and collection over other systems and permits continuous particle formation, in particular by dispersion of a solute-containing process fluid within a supercritical anti-solvent. 1. A particle formation and collection equipment assembly comprising:at least one high pressure particle formation system comprising a pressurizable precipitation chamber comprising a supercritical fluid (SCF) inlet, a process fluid inlet, a fluid outlet, a process fluid disperser configured to disperse process fluid into the chamber, wherein the system is configured to form a particle-containing high pressure liquid suspension; 'a) at least one high pressure harvesting filter system comprising at least one gas supply, at least one porous element, and a housing defining a cavity, wherein the filter system is configured to filter a particle-containing high pressure (compressed) liquid suspension;', 'at least one tandem particle filtration system comprising 'b) at least one low pressure collection filter system in tandem and downstream to the harvesting filter, wherein the filter system is configured to filter a particle-containing low pressure gaseous suspension; and', 'and'}at least one particle collection system comprising at least one collection vessel downstream to either filter.2. The equipment assembly of further comprising: a) one or more temperature controllers for one or more of the precipitation chamber claim 1 , collection filter ...

Transferring a target substance between two liquid phases

The invention relates to a method for transferring a target substance (5), particularly a target molecule (5), between two liquid phases (4, 6; 6, 8; 6, 11), of which at least one phase (4, 6) comprises the target substance (5) to be transferred and at least one phase (4, 8, 11) is an aqueous phase, where at least the aqueous phase (4, 8, 11) is arranged in one of two electrode chambers (1a, 1b, 10a, 10b) which are electroconductively connected, preferably by charge carrier exchange, and separated in terms of the volumes thereof, preferably where the phases (4, 6; 6, 8; 6, 11) are arranged together in one of two electrode chambers (1a, 1b, 10a, 10b) which are electroconductively connected and separated in terms of the volumes thereof, and a pH-value modification is generated by the H and/or OH ions created during the electrolysis in the aqueous phase (4, 8, 11), said modification initiating a transfer process of the target substance (5) between the phases (4, 6; 6, 8; 6, 11). The invention also relates to the use of the method for enrichment and subsequent isolation of the target substance (5).

DOTA SYNTHESIS

The present invention provides methods for the preparation of compounds useful in in vivo therapeutic and diagnostic applications. In particular, the present invention provides a method for the synthesis of 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid (DOTA) and also methods for the preparation of metal chelates of DOTA. 1. A method for the synthesis of 1 ,4 ,7 ,10-tetraazacyclododecane-1 ,4 ,7 ,10-tetraacetic acid (DOTA) , the method comprising:(a) reacting 1,4,7,10-tetraazacyclododecane (cyclen) with a halo-acetic acid and an excess of a base;(b) crystallising the reaction mixture obtained in step (a) wherein said crystallising is carried out at a pH>3 and <3.5;(c) filtering an aqueous solution of the crystallised product of step (b) using membrane filtration; and(d) crystallising the filtered solution obtained in step (c).2. The method of claim 1 , wherein said halo-acetic acid is selected from the group comprising iodoacetic acid claim 1 , bromoacetic acid and chloroacetic acid.3. The method of claim 1 , wherein said halo-acetic acid is chloroacetic acid.4. The method of claim 1 , wherein said halo-acetic acid is the salt of said halo-acetic acid.5. The method of claim 1 , wherein said base is selected from the group comprising an alkali hydroxide or an alkaline-earth metal hydroxide.6. The method of claim 1 , wherein said base is an alkali hydroxide.7. The method of claim 1 , wherein said base is NaOH or KOH.8. The method of claim 1 , wherein said base is NaOH.9. The method of claim 1 , wherein said base is KOH.10. The method of claim 1 , wherein step (a) is carried out at pH 9.0-12.5.11. The method of claim 1 , wherein step (a) is carried out at pH 9.5-12.0.12. The method of claim 1 , wherein step (a) is carried out at pH 10.0-11.5.13. The method of claim 1 , wherein step (a) is carried out at pH 10.5-11.5.14. The method of claim 1 , wherein step (a) is carried out at a pH of around 11.15. The method of claim 1 , wherein the pH in step (b) is ...

Rotor-stator apparatus and process for the formation of particles

The present invention relates to the use of a high intensity, in-line rotor-stator apparatus to produce fine particles via antisolvent, reactive, salting out or rapid cooling precipitation and crystallization.

制备晶体的方法

本发明公开了在存在超声波照射的条件下制备活性成分的晶体粒子的方法，该方法包括使在第一流动物流中的溶质在溶剂中的溶液接触在第二流动物流中的反溶剂，引发其混合，其中反溶剂∶溶剂的流速比高于20∶1，并收集产生的晶体。

PROCESS FOR THE PURIFICATION OF LITHIUM SALTS

A process for the recovery of lithium from waste lithium ion batteries or parts thereof is disclosed. The process comprising the steps of A) providing a crude lithium hydroxide as a solid, which contains fluoride; and (B) dissolving the crude lithium hydroxide solid with a lower alcohol such as methanol or ethanol provides good separation of lithium in high purity. 112-. (canceled)13. An electrode active material comprising{'sub': 1+x1', '1−x1', '2', '1, '(A) a core material according to general formula LiTMO, wherein TM is a combination of Ni and at least one of Mn, Co and Al, and, optionally, at least one more metal selected from Mg, Ti, Zr, Nb, Ta, and W, and xis in a range from −0.05 to 0.2, and'}(B) particles of cobalt compound(s), of aluminum compound(s), and of titanium compound(s) or of zirconium compound(s), wherein a molar ratio of lithium to cobalt in the particles is in a range of from zero to below 1, and wherein in the particles, a molar ratio of Co to the sum of Al and Zr or Ti is in a range from 2:1 to 50:1, and wherein the particles are attached to the surface of the core material.14. The electrode active material according to claim 13 , wherein TM is a combination of metals according to general formula (I){'br': None, 'sub': a', 'b', 'c', '1−d', 'd, '(NiCoMn)M\u2003\u2003(I)'}witha in a range of from 0.6 to 0.95,b in a range of from 0.025 to 0.2,c in a range of from 0.025 to 0.2, andd in a range of from zero to 0.1, {'br': None, 'i': 'a+b+c=', '1.'}, 'M is selected from Al, Mg, Ti, Zr, Nb, Ta, W, and combinations of at least two of the foregoing and'}15. The electrode active material according to claim 13 , wherein an average oxidation state of cobalt is higher than +II and lower than +III.16. The electrode active material according to claim 13 , wherein the particles comprise CoO.17. The electrode active material according to claim 13 , wherein a weight ratio of core (A) and particles (B) ranges from 1000:1 to 1 to 1.18. The electrode active ...

Process for producing solid material by precipitation

Verfahren zur Herstellung von Feststoffen durch Fällung in einem Mischer unter Bildung eines Gemisches aus Feststoff und Flüssigkeit, wobei man die Einsatzstoffe einer Mischvorrichtung (3) zuführt, welche im wesentlichen eine rotationssymmetrische Mischkammer mit darin angeordnetem Rotor aufweist, die aus einer Umfangswand und zwei Stirnwänden gebildet wird und wobei man a) die Einsatzstoffe mindestens je einer Einlaßöffnung in der Umfangswand der Mischkammer zuführt und b) das gebildete feststoffhaltige Gemisch mindestens einer Auslaßöffnung (7,11) in der Umfangswand in der Mischkammer entnimmt. Process for the production of solids by precipitation in a mixer to form a mixture of solid and liquid, the feed materials being fed to a mixing device (3) which essentially has a rotationally symmetrical mixing chamber with a rotor arranged therein, which is formed from a peripheral wall and two end walls and where one a) feeds at least one inlet opening in the peripheral wall of the mixing chamber and b) the solid-containing mixture formed takes at least one outlet opening (7, 11) in the peripheral wall in the mixing chamber.

Compositions of particulate coformulation

Embodiments of the invention provide a composition of a particulate coformulation which includes particles containing an active substance and an additive, wherein each particle contains a relative additive concentration increasing radially outwards from a particle center to a particle surface along a finite gradient. In one example, the particle surface is an additive-rich surface without a distinct physical boundary between the particle center and the particle surface. The relative additive concentration may have a continuous rate of change across the finite gradient. In some examples, an active substance:additive ratio of the particle surface is sufficiently low to form a protective surface layer around the active substance. Generally, the particle surface is free of the active substance.

Supercritical fluid-assisted nebulization and bubble drying

A method of making fine dry particles of substances is provided by forming a composition comprising a substance of interest and a supercritical or near critical fluid; rapidly reducing the pressure on said composition, whereby droplets are formed; and passing said droplets through a flow of heated gas. The process does not require any organic solvent.

Compositions of particulate coformulation

Embodiments of the invention provide a composition of a particulate coformulation which includes particles containing an active substance and an additive, wherein each particle contains a relative additive concentration increasing radially outwards from a particle center to a particle surface along a finite gradient. In one example, the particle surface is an additive-rich surface without a distinct physical boundary between the particle center and the particle surface. The relative additive concentration may have a continuous rate of change across the finite gradient. In some examples, an active substance: additive ratio of the particle surface is sufficiently low to form a protective surface layer around the active substance. Generally, the particle surface is free of the active substance.

Compositions of particulate coformulation

Embodiments of the invention provide a composition of a particulate coformulation which includes particles containing an active substance and an additive, wherein each particle contains a relative additive concentration increasing radially outwards from a particle center to a particle surface along a finite gradient. In one example, the particle surface is an additive-rich surface without a distinct physical boundary between the particle center and the particle surface. The relative additive concentration may have a continuous rate of change across the finite gradient. In some examples, an active substance:additive ratio of the particle surface is sufficiently low to form a protective surface layer around the active substance. Generally, the particle surface is free of the active substance.

Method and apparatus for preparation of lactide using lactide purification process

The present invention relates to a method and an apparatus for producing lactide using a lactide purification process. More specifically, provided is a method for producing lactide, which comprises: a step for carrying out a reaction after injection of an aqueous lactic acid solution into a catalyst-filled reactor, so as to generate lactide steam; and a first purification step for producing lactide crystals by purifying the lactide steam. The first purification step further comprises: a step for producing the lactide crystals by capturing and crystallizing lactide steam using a first solvent; and a step for separating the lactide crystals from residues through filtration.

Plinabulin compositions

Method of producing crystals

FIELD: process engineering. SUBSTANCE: invention relates to method of producing fine crystals. Method of producing crystalline particles of active component in the presence of ultrasound radiation comprises bringing solution of substance diluted in solvent in first current flow with anti-solvent for both to be mixed. Note here that relationship between flow rate of anti-solvent and flow rate of solvent exceeds 20:1. Further it comprises collecting formed crystals. EFFECT: crystals with necessary active component sized to 10 mcm. 60 cl, 6 dwg РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) 2 456 066 (13) C2 (51) МПК B01J 2/02 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ (21)(22) Заявка: 2009138325/05, 18.03.2008 (24) Дата начала отсчета срока действия патента: 18.03.2008 (72) Автор(ы): РОБИНСОН Джеймс (GB), РУКРОФТ Грехем (GB) (73) Патентообладатель(и): ПРОСОНИКС ЛИМИТЕД (GB) R U Приоритет(ы): (30) Конвенционный приоритет: 19.03.2007 GB 0705159.2 (43) Дата публикации заявки: 27.04.2011 Бюл. № 12 2 4 5 6 0 6 6 (45) Опубликовано: 20.07.2012 Бюл. № 20 (56) Список документов, цитированных в отчете о поиске: WO 03061816 A1, 31.07.2003. WO 0038811 A1, 06.07.2000. RU 2125869 C1, 10.02.1999. RU 2232629 C2, 20.07.2004. RU 2033254 C1, 20.04.1995. 2 4 5 6 0 6 6 R U (86) Заявка PCT: GB 2008/050191 (18.03.2008) C 2 C 2 (85) Дата начала рассмотрения заявки PCT на национальной фазе: 19.10.2009 (87) Публикация заявки РСТ: WO 2008/114052 (25.09.2008) Адрес для переписки: 129090, Москва, ул. Б. Спасская, 25, стр.3, ООО "Юридическая фирма Городисский и Партнеры" (54) СПОСОБ ПОЛУЧЕНИЯ КРИСТАЛЛОВ (57) Реферат: Изобретение относится к способу получения мелких кристаллов. Способ получения кристаллических частиц активной составляющей в присутствии ультразвукового излучения включает контактирование раствора растворенного вещества в растворителе в первом текущем потоке с анти-растворителем во втором текущем потоке, вызывающее их смешение, в котором ...

Conditioning amine solvent contaminated with introduced sulphur oxides

FIELD: chemistry. SUBSTANCE: invention refers to a method and a device for conditioning an amine solvent contaminated with introduced sulphur dioxides. The contaminated solvent is added with a potassium compound and an oxidising agent thereby oxidising sulphite to sulphate; the oxidising agent and potassium compound are mixed before adding an amino acid salt to the solution. The contaminated solvent is cooled down to a temperature T, thereby reducing the potassium sulphate solubility as compared to its actual concentration. Potassium sulphate is filtered to produce the conditioned solvent. EFFECT: invention enables providing removing sulphate from the solution. 15 cl, 3 dwg РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2 559 493 C2 (51) МПК B01D 53/14 (2006.01) B01D 53/50 (2006.01) B01D 9/00 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ОПИСАНИЕ (21)(22) Заявка: ИЗОБРЕТЕНИЯ К ПАТЕНТУ 2013126536/05, 08.11.2011 (24) Дата начала отсчета срока действия патента: 08.11.2011 Приоритет(ы): (30) Конвенционный приоритет: (43) Дата публикации заявки: 20.12.2014 Бюл. № 35 (73) Патентообладатель(и): СИМЕНС АКЦИЕНГЕЗЕЛЛЬШАФТ (DE) R U 10.11.2010 DE 102010043689.5 (72) Автор(ы): ФОРБЕРТ Райнальд (DE), ХАУКЕ Стефан (DE), ЙОХ Ральф (DE), ОЛЬШЕВСКИ Франк (DE), ШНАЙДЕР Рюдигер (DE) (45) Опубликовано: 10.08.2015 Бюл. № 22 (85) Дата начала рассмотрения заявки PCT на национальной фазе: 10.06.2013 2 5 5 9 4 9 3 (56) Список документов, цитированных в отчете о поиске: US 20040253159 А1, 16.12.2004. US 5853012 А, 19.05.1998. US 4500500 A, 19.02.1985. SU 795448, 08.01.1981. US 4389383 A, 21.06.1983. DE 2702583 A1, 27.07.1978. US 5912387 A, 15.06.1999. US 6010664 A, 04.01.2000 EP 2011/069593 (08.11.2011) C 2 C 2 (86) Заявка PCT: (87) Публикация заявки PCT: R U 2 5 5 9 4 9 3 WO 2012/062724 (18.05.2012) Адрес для переписки: 109012, Москва, ул. Ильинка, 5/2, ООО "Союзпатент" (54) ОЧИСТКА ЗАГРЯЗНЁННОГО ВНЕСЕНИЕМ ОКСИДОВ СЕРЫ РАСТВОРИТЕЛЯ НА ОСНОВЕ АМИНА (57) Реферат: Изобретение ...

The method for preparing crystal

本发明公开了在存在超声波照射的条件下制备活性成分的晶体粒子的方法，该方法包括使在第一流动物流中的溶质在溶剂中的溶液接触在第二流动物流中的反溶剂，引发其混合，其中反溶剂∶溶剂的流速比高于20∶1，并收集产生的晶体。

Method for producing crystalline active ingredient particles

本发明涉及一种晶体活性成分颗粒的制备方法，其中活性成分从过饱和溶液于该活性成分颗粒的表面上结晶出来，其中在一第一模块中，在该活性成分的过饱和溶液中对活性成分颗粒的悬浮液进行湿磨，至少部分活性成分颗粒的悬浮液于一第二模块中被冷却并且同时经过超声波处理，在该第二模块内提供有来自该第一模块的该活性成分颗粒悬浮液，并且在冷却并经超声波处理之后，该活性成分颗粒悬浮液再提供回该第一模块内，其中将活性成分溶液及可选择性的抗溶剂添加至该悬浮液，并且提取活性成分颗粒以及液相，其中相对于总液相，该悬浮液的液相中活性成分的相对过饱和度为小于等于90％，并且被提取的活性成分颗粒包括10-500μm的平均粒径d 50 。

Crystalline form of maleate of condensed pyridine derivative and methods for use thereof

FIELD: chemistry.SUBSTANCE: invention relates to a crystalline form of a maleate salt of N-(4-(2,3-dihydro-1H-pyrrolo[2,3-b]pyridin-4-yloxy)-3-fluorophenyl)-5-(4-fluorophenyl)-4-oxo-1,4-dihydropyridine-3-carboxamide of formula (I), where its X-ray powder pattern is characterized by characteristic peaks at diffraction angles 2θ at values of 8.6° ± 0.2°, 15.8° ± 0.2°, 16.5° ± 0.2°, 19.5° ± 0.2°, 20.2° ± 0.2° and 26.5° ± 0.2°; wherein powder X-ray diffraction pattern is obtained using X-ray diffraction system D8-Advance and K-alpha radiation of copper anode of X-ray tube as radiation source. Method of producing a crystalline form of formula I involves reacting a compound of formula II with maleic acid in a reaction medium based on ethyl acetate in a glass reactor at room temperature, centrifuging and drying overnight under vacuum at room temperature to obtain the desired crystalline form.EFFECT: crystalline maleate salt of N-(4-(2,3-dihydro-1H-pyrrolo[2,3-b]pyridin-4-yloxy)-3-fluorophenyl)-5-(4-fluorophenyl)-4-oxo-1,4-dihydropyridine-3-carboxamide is intended for preparing a drug preparation or pharmaceutical composition for treating a c-Met-mediated disorder.14 cl, 3 tbl, 3 dwg, 13 ex РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2 712 280 C2 (51) МПК C07D 487/04 (2006.01) C07D 401/14 (2006.01) A61K 31/437 (2006.01) A61P 35/00 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ (52) СПК C07D 487/04 (2019.05); C07D 401/14 (2019.05); A61K 31/437 (2019.05); A61P 35/00 (2019.05) (21)(22) Заявка: 2018106101, 20.07.2016 (24) Дата начала отсчета срока действия патента: Дата регистрации: 28.01.2020 20.07.2015 CN PCT/CN2015/084414 (43) Дата публикации заявки: 20.08.2019 Бюл. № 23 (45) Опубликовано: 28.01.2020 Бюл. № 4 (85) Дата начала рассмотрения заявки PCT на национальной фазе: 20.02.2018 (56) Список документов, цитированных в отчете о поиске: WO 2014/000713 A1, 03.01.2014. WO 2012/006960 A1, 19.01.2012. WO 2006/014325 A2, 09.02.2006 . ...

Method and apparatus for continuous post-treatment of penem-based compounds

페넴계 화합물 연속 후처리 방법 및 장치를 제공한다. 상기 방법은, 페넴계 화합물의 반응 조 생성물을 연속 추출하여, 추출 중상 및 추출 경상을 얻는 단계 S1; 추출 중상에 대해 연속 고액 분리를 수행하여, 액상 분리물을 얻는 단계 S2; 액상 분리물에 대해 그 pH 값이 6.1~6.3이 될 때까지 연속 pH 조절을 수행하여, pH 조절액을 얻는 단계 S3; 및 제1 결정화 용매를 사용하여 pH 조절액에 대해 연속 결정화 처리를 수행하여, 페넴계 화합물의 제품을 얻는 단계 S4를 포함한다. 상기 방법을 사용하여 페넴계 화합물의 반응 조 생성물에 대해 후처리를 진행하면 처리 속도가 빠르고 효율이 높은 이점이 있고, 처리 공정에서 재료 성질이 안정적이고 변질율이 낮으며 목적 생성물의 수율 및 순도에 대한 제어 능력이 더 좋다.

Lithium carbonate manufacturing method

Patent RU2018106101A3

РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2018 106 101 A (51) МПК C07D 487/04 (2006.01) C07D 401/14 (2006.01) A61K 31/437 (2006.01) A61P 35/00 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ЗАЯВКА НА ИЗОБРЕТЕНИЕ (21)(22) Заявка: 2018106101, 20.07.2016 (71) Заявитель(и): БЕТТА ФАРМАСЬЮТИКАЛЗ КО., ЛТД (CN) Приоритет(ы): (30) Конвенционный приоритет: 20.07.2015 CN PCT/CN2015/084414 (85) Дата начала рассмотрения заявки PCT на национальной фазе: 20.02.2018 (86) Заявка PCT: (87) Публикация заявки PCT: WO 2017/012539 (26.01.2017) A Адрес для переписки: 123242, Москва, Кудринская пл., 1, а/я 35, "Михайлюк, Сороколат и партнеры-патентные поверенные" R U (57) Формула изобретения 1. Кристаллическая форма соединения формулы I, A 2 0 1 8 1 0 6 1 0 1 (54) КРИСТАЛЛИЧЕСКАЯ ФОРМА МАЛЕАТА КОНДЕНСИРОВАННОГО ПИРИДИНОВОГО ПРОИЗВОДНОГО И СПОСОБЫ ЕЕ ПРИМЕНЕНИЯ 2 0 1 8 1 0 6 1 0 1 CN 2016/090613 (20.07.2016) R U (43) Дата публикации заявки: 20.08.2019 Бюл. № 23 (72) Автор(ы): ХУ Шаоцзин (CN), ЛУН Вэй (CN), ЧЖОУ Люфэн (CN), СЮЙ Чжигоу (CN), ВАН Фэй (CN) Формула I, где ее порошковая рентгенограмма характеризуется характеристическими пиками при дифракционных углах 2θ при значениях 8,6°±0,2°, 16,5°±0,2° и 26,5°±0,2°. 2. Кристаллическая форма по п. 1, где ее порошковая рентгенограмма характеризуется характеристическими пиками при дифракционных углах 2θ при значениях 8,6°±0,2°, 15,8°±0,2°, 16,5°±0,2°, 19,5°±0,2°, 20,2°±0,2° и 26,5°±0,2°. 3. Кристаллическая форма по любому из пп. 1-2, где ее порошковая рентгенограмма характеризуется характеристическими пиками при дифракционных углах 2θ при значениях 8,6°±0,2°, 10,5°±0,2°, 15,8°±0,2°, 16,5°±0,2°, 19,5°±0,2°, 20,2°±0,2°, 23,6°±0,2°, 26,5°±0,2° и 29,1°±0,2°. Стр.: 1 2 0 1 8 1 0 6 1 0 1 R U A Стр.: 2 2 0 1 8 1 0 6 1 0 1 Формула II, с малеиновой кислотой в реакционной среде на основе этилацетата в стеклянном реакторе при комнатной температуре, центрифугирование и высушивание в течение ночи под вакуумом при комнатной температуре с ...

Microparticle manufacturing method

미립자의 제조 방법을 제공하는 것을 과제로 한다. 미립자의 제조 방법을 제공한다. 제 1 공정으로서 대향해서 배치되고, 접근·이반 가능하고, 적어도 한쪽이 다른쪽에 대하여 상대적으로 회전하는 적어도 2개의 처리용 면 사이에 생성되는 박막 유체 중에 있어서 시드 미립자를 석출시키고, 석출시킨 시드 미립자를 포함하는 유체를 토출액으로서 배출시킨다. 그 후, 제 2 공정으로서 배출시킨 토출액 중에 있어서 석출시킨 시드 미립자를 성장시켜서 목적의 미립자를 얻는다. 미립자의 제조 방법에 있어서 상기 2공정을 포함함으로써 균일하며 또한 균질한 미립자를 얻는다. And to provide a method for producing fine particles. A method for producing fine particles is provided. The seed microparticles are precipitated in the thin film fluid which is disposed opposite to the first process and is accessible and transferable and is formed between at least two processing surfaces in which at least one of them rotates relative to the other side, And discharges the contained fluid as a discharge liquid. Thereafter, the seed fine particles precipitated in the discharged liquid discharged as the second step are grown to obtain desired fine particles. In the method for producing fine particles, homogeneous and homogeneous fine particles are obtained by including the above two steps.

Process for the production of a therapeutically effective extract from the cement resin of the Apis mellifica

Process for the preparation of amorphous idelalisib and its premix

Processes for the preparation of amorphous idelalisib are provided. Processes for the preparation of a premix of amorphous idelalisib are also provided.

Gas-phase antimicrobial delivery via infused crystalline and porous solids

Methods and systems are provided for infusing a crystalline and/or porous solid with a desired fluid, particularly an antimicrobial agent, as well as infused crystalline and/or porous solids produced thereby. Solids which may be infused with an antimicrobial agent according to the invention include erythritol, table salt, table sugar, baking soda, calcium carbonate, acetic acid, ascorbic acid, and marshmallow.

Method for producing a mixed metal solution and a method for producing a mixed metal salt

망간 이온과, 코발트 이온 및 니켈 이온 중 적어도 1종을 포함하는 금속 혼합 용액을 제조하는 방법이며, 리튬 이온 전지 폐기물의 전지분을 침출 공정에 제공해서 얻어진 산성 용액이며, 적어도 망간 이온 및 알루미늄 이온과, 코발트 이온 및 니켈 이온 중 적어도 1종을 포함하는 당해 산성 용액에 대해서, 상기 산성 용액 중의 망간 이온의 적어도 일부를 수상에 잔류시키면서, 알루미늄 이온을 용매로 추출해서 제거하는 Al 제거 공정과, 상기 Al 제거 공정에서 얻어지는 추출 잔액에 대하여, 카르복실산계 추출제를 포함하는 용매를 사용해서 평형 pH를 6.5 내지 7.5로 하고, 추출 잔액 중의 망간 이온과 코발트 이온 및 니켈 이온 중 적어도 1종을 당해 용매로 추출한 후, 당해 용매로부터 망간 이온과 코발트 이온 및 니켈 이온 중 적어도 1종을 역추출하는 금속 추출 공정을 포함한다.

Method for efficiently extracting and separating high-purity tetrodotoxin from globefish viscera

本发明公开一种高效的从河豚内脏提取和分离制备高纯度河豚毒素（tetrodotoxin,简称TTX）的方法；其包括以下步骤：将干净的河豚内脏加酸性醇匀浆、加入一定量的助流动剂搅拌均匀后，按柱层析的装柱方法将材料装入层析柱中；用同一酸性醇将河豚内脏中的TTX完全洗脱出来，收集洗脱液为TTX提取液；提取液减压浓缩至水相，得到TTX提取浓缩液；TTX水溶液用离子交换树脂柱层析分离，收集含TTX高的洗脱液，用纳滤膜浓缩或减压蒸干，得到TTX粗品；TTX粗品通过溶剂沉淀和结晶，得到纯度达于98%的TTX；本发明的制备TTX的方法和所用设备简单，TTX提取和分离纯化的得率高、制备成本低，适合TTX的规模化生产；同时该方法使用的有机溶剂可全部回收重复使用，无有害溶剂和废弃物排放，是理想的安全环保的制备TTX方法。

Process for the selective recovery of transition metals from organic residues

The present invention relates to a process for the selective recovery of transition metals from an organic stream containing transition metals. The organic stream and possibly a first extractor if solid, are melted up to the liquid state. The extractor consists of an ionic liquid or a mixture of two or more ionic liquids, wherein said ionic liquid contains an ammonium salt as cation and as anion an anion with chelating properties. A melted organic stream and a first extractor, optionally melted, are fed to a first liquid-liquid extraction unit working at a temperature of at least 150 °C where the liquid-liquid extraction is carried out obtaining a liquid mixture containing an ionic liquid, or a mixture of two or more ionic liquids, and metals. After extraction, the liquid mixture is cooled at a temperature between 0 °C and 70 °C and becomes biphasic; then the cooled mixture is sent to a first separation unit, to separate a liquid phase that contains ionic liquids and metals, and a metal-depleted solid phase. After the first separation, the separated metal-depleted solid phase is optionally sent to a washing unit to which a solvent is fed, so as to eliminate the residual ionic liquid by transferring it into the solvent and obtaining a metal-depleted solid phase. Then the separate liquid phase containing ionic liquids and metals is sent into a liquid-liquid precipitation and separation unit, adding a counter-solvent, thereby obtaining a solid phase containing the metals and a liquid stream containing counter-solvent and ionic liquids.

Methods of preparing solid particulate materials

There is described a method of preparing solid particles of a compound, said method comprising controlling provision of a liquid phase, wherein said liquid phase comprises a solution of the compound, in a first flow direction to a membrane, said membrane defining a plurality of pores; and controlling the supersaturation of the liquid phase after it has passed through the membrane via the plurality of pores, to form solid particles of the compound. The method may comprise a continuous method.

Process for preparation of dapagliflozin

The present invention relates to a process for the preparation of amorphous dapagliflozin. The present invention relates to 2,3-butanediol solvate of dapagliflozin and process for its preparation.