Hydrogenation process for the preparation of tetrahydrofuran and alkylated derivatives thereof

A process is provided for the synthesis of tetrahydrofuran and related compounds by hydrogenation of furan and derivatives, using a sponge nickel catalyst that has been promoted with iron and chromium.

METHOD AND INTERMEDIATE FOR PREPARING TULATHROMYCIN

A method and an intermediate for preparing a tulathromycin. The method includes the following step: in an organic solvent, subjecting a compound represented by formula (II) and an n-propylamine to a ring-opening addition shown below to obtain a tulathromycin represented by formula (I), wherein the organic solvent is a 1,2-propandiol. Tulathromycin obtained using the method has a high purity, with an HPLC purity being 95% and above, and up to 99% and above, satisfying a required purity for preparing a tulathromycin as a pharmaceutical formulation. The method has a high yield, is simple to operate, and is more suitable for industrial production. 2. The method according to claim 1 , wherein the mole ratio of the compound represented by formula II to n-propylamine is preferably from 1:5 to 1:30 claim 1 , more preferably from 1:8 to 1:15; the temperature of the ring-opening addition reaction is preferably between 30 and 90° C. claim 1 , more preferably between 40 and 65° C. claim 1 , and most preferably between 45 and 55° C.; the duration of the ring-opening addition reaction is preferably from 15 to 40 hours claim 1 , and more preferably from 16 to 20 hours; the method for preparing tulathromycin represented by formula I preferably comprises the following steps: mixing a mixed solution of the compound represented by formula II and the organic solvent with n-propylamine claim 1 , and performing the ring-opening addition reaction; the ring-opening addition reaction is preferably performed in the condition of gas protection; the gas for the gas protection is preferably nitrogen.3. The method according to claim 1 , which further comprises a post-processing treatment after the completion of the ring-opening addition reaction; the post-processing treatment comprises the following steps: removing n-propylamine and the organic solvent after the completion of the ring-opening addition reaction to obtain crude tulathromycin represented by formula I; and performing ...

METHOD FOR PRODUCING TETRAHYDROFURAN

The present invention relates to a method for producing tetrahydrofuran comprising: feeding raw material 1,4-butanediol containing gamma butyrolactone to a reaction tank, and performing a dehydration cyclization reaction in the presence of a homogeneous acid catalyst having a pKa of 4 or less and being dissolvable in 1,4-butanediol to produce tetrahydrofuran, wherein a gas containing tetrahydrofuran, gamma butyrolactone and water in the reaction tank is introduced into a heat exchanger and when obtaining a condensate from the outlet of the heat exchanger, the ratio of the concentration of gamma butyrolactone in the condensate based on the concentration of gamma butyrolactone in the raw material 1,4-butanediol is from 20 to 100%. 1. A method for producing tetrahydrofuran , comprising feeding raw material 1 ,4-butanediol containing gamma butyrolactone to a reaction tank , and performing a dehydration cyclization reaction in the presence of a homogeneous acid catalyst having a pKa of 4 or less and being dissolvable in 1 ,4-butanediol to produce tetrahydrofuran , wherein a gas containing tetrahydrofuran , gamma butyrolactone and water in the reaction tank is introduced into a heat exchanger and when obtaining a condensate from the outlet of the heat exchanger , the ratio of the concentration of gamma butyrolactone in the condensate based on the concentration of gamma butyrolactone in the raw material 1 ,4-butanediol is from 20 to 100%.2. The production method of tetrahydrofuran according to claim 1 , wherein the temperature of a liquid phase part in the reaction tank is from 80 250° C.3. The production method of tetrahydrofuran according to claim 1 , wherein the concentration of the homogeneous acid catalyst in the reaction tank is from 0.01 to 20.0 wt %.4. The production method of tetrahydrofuran according to claim 1 , wherein the homogeneous acid catalyst is mixed with and dissolved in the raw material 1 claim 1 ,4-butanediol and then fed to the reaction tank.5. The ...

Process for the Oxidation of Organic Carbonyl Compounds

A process for the oxidation of an organic carbonyl compound comprising reacting the organic carbonyl compound, optionally in the presence of a solvent, with hydrogen peroxide in the presence of a catalyst comprising a tin-containing zeolitic material having an MWW-type framework structure. 2. The process of claim 1 , wherein Rand Rare independently from one another a linear or branched alkyl residue having from 1 to 20 carbon atoms claim 1 , a linear or branched alkenyl residue having from 2 to 20 carbon atoms claim 1 , an aryl or heteroaryl residue having from 4 to 20 carbon atoms claim 1 , or a hydrogen atom and wherein claim 1 , if neither Rnor Ris a hydrogen atom claim 1 , Rand Rmay form claim 1 , together with the carbonyl group or the carboxyl group claim 1 , a ring having from 4 to 20 carbon atoms.3. The process of claim 1 , wherein the compound of formula (I) contains at least one C—C double bond.4. The process of claim 3 , wherein the compound of formula (I) contains a C—C double bond in alpha position to the carbonyl group.5. The process of claim 1 , wherein at least 99 weight-% of the framework structure of the Sn-MWW consist of BOand SiO claim 1 , wherein the molar ratio of BOrelative to SiOis in the range of from 0.0005:1 to 0.0025:1.6. The process of claim 1 , wherein the Sn-MWW has a tin content in the range of from 0.1 to 4.0 weight-% claim 1 , calculated as element and based on the weight of the Sn-MWW.7. The process of claim 1 , wherein the Sn-MWW has a tin content in the range of from 0.1 to 1.0 weight-% or in the range of from 0.1 to 0.5 weight-% claim 1 , calculated as element and based on the weight of the Sn-MWW.8. The process of claim 1 , wherein at the beginning of the reaction according to (i) claim 1 , the molar ratio of Sn claim 1 , calculated as element and contained in the Sn-MWW claim 1 , relative to the compound according to formula (I) is in the range of from 0.001:1 to 0.05:1.9. The process of claim 1 , wherein at the beginning of ...

METHODS FOR PRODUCING TETRAHYDROFURAN

The present disclosure provides a method for producing tetrahydrofuran (THF). The method includes: feeding 1,4-butanediol into a reactive distillation apparatus; performing the dehydration reaction in the presence of an acidic catalyst; and producing the top stream containing product THF and the bottom stream from the reactive distillation apparatus, wherein a weight ratio of a water content in the bottom stream to a water content in the top stream is 0.05 to 2.4, thereby providing a high conversion rate and more cost-effectiveness, and enhancing the value of the industrial application. 1. A method for producing tetrahydrofuran , comprising:feeding a reactant stream containing 1,4-butanediol into a reactive distillation apparatus, and performing a dehydration reaction in a presence of an acidic catalyst to produce a top stream containing tetrahydrofuran and a bottom stream from the reactive distillation apparatus, wherein a weight ratio of a water content in the bottom stream to a water content in the top stream is from 0.05 to 2.4.2. The method of claim 1 , wherein the reactive distillation apparatus comprises claim 1 , from top to bottom claim 1 , a rectification section and a reactive section claim 1 , and wherein the reactive section is packed with the acidic catalyst.3. The method of claim 1 , wherein the reactant stream containing 1 claim 1 ,4-butanediol has a weight hourly space velocity (WHSV) of from 2.1 to 2.5 hr.4. The method of claim 2 , wherein the rectification section has 10 to 20 plates claim 2 , and the reactive section has 40 to 60 plates.5. The method of claim 4 , wherein the reactant stream containing 1 claim 4 ,4-butanediol is fed into the uppermost plate in the reactive section.6. The method of claim 5 , wherein a water content at the uppermost plate in the reactive section is from 1.6 to 13 wt % claim 5 , and a water content at the lowermost plate in the reactive section is from 67 to 94 wt %.7. The method of claim 2 , wherein the ...

METHOD FOR PRODUCING TETRAHYDROFURAN

The present invention is concerned with a method for producing tetrahydrofuran including carrying out a dehydration cyclization reaction of 1,4-butanediol in the presence of an acid catalyst having a pKa value of not more than 4 within a reactor, wherein a raw material liquid containing 1,4-butanediol to be provided for the reaction contains from 0.01 to 0.35% by weight of 2-(4-hydroxybutoxy)-tetrahydrofuran and 1 ppm by weight or more and not more than 1,000 ppm by weight of at least one of an amine and an amide in terms of a concentration as converted into a nitrogen atom. 1. A method for producing tetrahydrofuran , comprising:carrying out a dehydration cyclization reaction of 1,4-butanediol in a presence of an acid catalyst having a pKa value of not more than 4 within a reactor,wherein a raw material liquid containing 1,4-butanediol to be provided for the reaction contains from 0.01 to 0.35% by weight of 2-(4-hydroxybutoxy)-tetrahydrofuran and 1 ppm by weight or more and not more than 1,000 ppm by weight of at least one of an amine and an amide in terms of a concentration as converted into a nitrogen atom.2. A method for producing tetrahydrofuran , comprising:carrying out a dehydration cyclization reaction of 1,4-butanediol in a presence of an acid catalyst having a pKa value of not more than 4 within a reactor,wherein a reaction liquid within the reactor contains 1 ppm by weight or more and not more than 10,000 ppm by weight of at least one of an amine and an amide in terms of a concentration as converted into a nitrogen atom.3. The method for producing tetrahydrofuran according to claim 1 ,wherein a reaction liquid within the reactor contains 1 ppm by weight or more and not more than 10,000 ppm by weight of at least one of an amine and an amide in terms of a concentration as converted into a nitrogen atom.4. The method for producing tetrahydrofuran according to claim 1 ,wherein a reaction liquid within the reactor contains 0.1% by weight or more and not more ...

Vascular Constructs

The invention is directed to products and methods for preparing self-seeding vascular constructs generated as a bi-layered electrospun matrices, conjugated with EPC-specific antibodies and anti-thrombogenic agents on the inner surfaces of their lumens. 1. A method of preparing a vascular construct by an electrospinning process , comprising:electrically charging a solution of a matrix material;discharging the electrically charged solution onto a grounded target under an electrostatic field to produce fibers of the matrix on the grounded target, wherein the matrix has a tubular shape and a three-dimensional ultrastructure of interconnected fibers with pores to permit cell attachment;manipulating the electrospinning process parameters to vary the porosity of the matrix to form multiple layers having different porosities such that the tubular matrix comprises an inner region, in which the average pore size is less than 1 micron and an outer region, in which the average pore size is greater than 1 micron; andconjugating one or more EPC-specific antibodies or one or more anti-thrombogenic agents to a surface of the three-dimensional ultrastructure.2. The method of claim 1 , wherein the step of manipulating the process parameters further comprises varying the fiber size claim 1 , whereby a bi-layered matrix is formed.3. The method of claim 1 , wherein the step of manipulating the process parameters further comprises varying the electrospinning process parameters such that the tubular matrix has an inner region claim 1 , in which the average pore size is between 100 and 900 nanometers and an outer region claim 1 , in which the average pore size is between 1 micron and 10 microns.4. The method of claim 1 , wherein the step of manipulating the process parameters further comprises varying the electrospinning process parameters such that the tubular matrix has an inner region claim 1 , in which the average pore size is between 200 and 700 nanometers and an outer region claim 1 ...

IMPROVED PROCESS FOR MANUFACTURE OF TETRAHYDROFURAN

The disclosed process relates to an improved process for manufacturing THF from a reaction mixture comprising BDO in the presence of an acid catalyst in a reaction vessel comprising a distillation reaction zone, wherein the acid catalyst is suspended in a vapor-rich region in the distillation reaction zone. 1. An improved process for making tetrahydrofuran , the process comprising:providing a reaction mixture comprising 1,4-butanediol to a first zone;maintaining conditions of temperature and pressure in the first zone sufficient to produce a vapor-rich region comprising the reaction mixture;providing a second zone in the vapor-rich region between the first zone and a vapor condenser, wherein the second zone comprises an acid catalyst;maintaining conditions of temperature and pressure in the second zone sufficient to effect dehydration of 1,4-butanediol and ring closure to form a product comprising tetrahydrofuran; andrecovering the product.2. The process of claim 1 , wherein the acid catalyst is a solid catalyst.3. The process of claim 2 , wherein the solid catalyst is selected from the group consisting of a polymer-based acid resin claim 2 , a mineral-based supported acid catalyst and combinations thereof.4. The process of claim 2 , wherein the solid catalyst is an acidic resin catalyst.5. The process of claim 4 , wherein the acidic resin catalyst has an acid equivalency of between 1 and 10.6. The process of claim 1 , wherein the temperature of the second zone is from 80 to 250° C.7. The process of claim 1 , wherein the product is comprised of 80±20/20±20 claim 1 , weight/weight claim 1 , tetrahydrofuran/water.8. The process of claim 6 , wherein the temperature of the second zone is from 110 to 250° C.9. The process of claim 1 , wherein the conditions of the second zone include a temperature of from 80 to 250° C. and pressure of from 200 to 10 claim 1 ,000 mbar absolute.10. The process of claim 9 , wherein the conditions of the second zone include a temperature of ...

METHOD FOR PRODUCING TETRAHYDROFURAN

The present invention relates to a method for producing tetrahydrofuran, comprising feeding 1,4-butanediol to a reactor and performing a cyclodehydration reaction in the presence of an acid catalyst to obtain tetrahydrofuran, in which a water concentration in a in-reactor liquid phase is within a range of 1.4 to 10 wt %. 2. The method for producing tetrahydrofuran as claimed in claim 1 , wherein said 1 claim 1 ,4-butanediol contains from 0.001 to 5.0 wt % of 2-(4-hydroxybutoxy)-tetrahydrofuran.3. The method for producing tetrahydrofuran as claimed in claim 1 , wherein the cyclodehydration reaction is performed by a reaction distillation method.4. The method for producing tetrahydrofuran as claimed in claim 1 , wherein said acid catalyst has a pKa value of 4 or less.5. The method for producing tetrahydrofuran as claimed in claim 1 , wherein said acid catalyst is a homogeneous acid catalyst.6. The method for producing tetrahydrofuran as claimed in claim 1 , wherein the acid catalyst concentration in said reactor liquid phase is controlled to a range from 0.01 to 20 wt %.7. The method for producing tetrahydrofuran as claimed in claim 1 , wherein the temperature of the liquid phase portion in said reactor is within a range of 80 to 250° C.8. The method for producing tetrahydrofuran as claimed in claim 1 , wherein said acid catalyst is an organic sulfonic acid.9. The method for producing tetrahydrofuran as claimed in claim 1 , further comprising a step of dissolving said acid catalyst having a pKa value of 4 or less in 1 claim 1 ,4-butanediol claim 1 , tetrahydrofuran or water and feeding the solution to the reactor.10. The method for producing tetrahydrofuran as claimed in claim 1 , wherein the viscosity at 25° C. of the solution of the liquid phase portion in said reactor is within a range of 50 to 1 claim 1 ,300 mPa·s.11. The method for producing tetrahydrofuran as claimed in claim 1 , wherein the water concentration in the liquid phase in said reactor is within a ...

Continuous Processing Method of 2-methyltetrahydrofuran

The disclosure claims a continuous processing method of 2-Methyltetrahydrofuran (2-MeTHF), including the steps as follows: introducing gasification furfural and hydrogen into a first reaction zone and processing a first catalytic hydrogenation reaction; introducing the gas which is output from the first reaction zone to a second reaction zone to implement a secondary catalytic hydrogenation reaction; and condensing the gas output from the second reaction zone to obtain the 2-MeTHF; wherein, the first reaction zone is filled with a catalyst which is used for aldehyde group reduction, and the second reaction zone is filled with the catalyst for aromatic saturation hydrogenation. By adopting the low-toxicity catalyst which is cheap and easy to get, the high-purity 2-MeTHF can be produced by implementing the gas-phase continuous reaction by the furfural under low pressure or ambient pressure, the traditional process which has high pressure, high investment and high risk can be changed. 1. A continuous processing method of 2-Methyltetrahydrofuran (2-MeTHF) , comprising the steps as follows:introducing gasification furfural and hydrogen into a first reaction zone and processing a first catalytic hydrogenation reaction;introducing the gas output from the first reaction zone into a second reaction zone and processing a secondary catalytic hydrogenation reaction; andcondensing the gas output from the second reaction zone to obtain the 2-MeTHF;wherein the first reaction zone is filled with a catalyst which is used for aldehyde group reduction, and the second reaction zone is filled with the catalyst which is used for aromatic saturation hydrogenation.2. The method according to claim 1 , wherein claim 1 ,before introducing the gasification furfural and the hydrogen into the first reaction zone, further comprising a step of premixing the gasification furfural and the hydrogen.3. The method according to claim 2 , wherein claim 2 ,before the secondary catalytic hydrogenation ...

RADIATION-SENSITIVE RESIN COMPOSITION, RESIST PATTERN-FORMING METHOD, ACID DIFFUSION CONTROL AGENT, COMPOUND, AND METHOD FOR PRODUCING COMPOUND

A radiation-sensitive resin composition includes a polymer including a structural unit that includes an acid-labile group; and a compound represented by formula (1). Rrepresents a monovalent organic group having 1 to 30 carbon atoms. L represents a single bond, an oxygen atom or a sulfur atom. M represents a monovalent radioactive ray-labile onium cation. The monovalent organic group represented by Ris preferably a monovalent hydrocarbon group or a monovalent fluorinated hydrocarbon group, and L preferably represents a single bond. The monovalent organic group represented by Ris preferably a monovalent hydrocarbon group, a monovalent fluorinated hydrocarbon group, a monovalent aliphatic heterocyclic group or a monovalent fluorinated aliphatic heterocyclic group, and L preferably represents an oxygen atom or a sulfur atom. The monovalent radioactive ray-labile onium cation represented by M is preferably represented by the formula (X). 2. The radiation-sensitive resin composition according to claim 1 , wherein the monovalent organic group represented by Rin the formula (1) is a monovalent hydrocarbon group or a monovalent fluorinated hydrocarbon group claim 1 , and L represents the single bond.3. The radiation-sensitive resin composition according to claim 1 , wherein the monovalent organic group represented by Rin the formula (1) is a monovalent hydrocarbon group claim 1 , a monovalent fluorinated hydrocarbon group claim 1 , a monovalent aliphatic heterocyclic group or a monovalent fluorinated aliphatic heterocyclic group claim 1 , and L represents the oxygen atom or the sulfur atom.5. The radiation-sensitive resin composition according to claim 1 , further comprising a radiation-sensitive acid generator.8. A resist pattern-forming method comprising:{'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, 'providing a resist film using the radiation-sensitive resin composition according to ;'}exposing the resist film; anddeveloping the exposed resist film. The present ...

SINGLE STEP PROCESS FOR CONVERSION OF FURFURAL TO TETRAHYDROFURAN

The present patent discloses a one step process for the synthesis of THF and related ring hydrogenated products form furfural using Palladium metal based carbon supported catalyst with high selectivity and 100% conversion in both batch and continuous modes. 1. A one step process for the synthesis of Tetrahydrofuran (THF) from furfural in both batch and continuous modes comprising: reacting furfural at a concentration in the range of 5 to 20% in the presence of Palladium metal based carbon supported catalyst at a concentration in the range of 5 to 20% at a temperature in the range of 423-513 K in presence of hydrogen at an elevated pressure to obtain THF with 10% to 41% selectivity and related ring hydrogenated products , wherein conversion percentage of furfural is 100%.2. The process according to claim 1 , wherein the concentration of furfural is 5% by weight.3. The process according to claim 1 , wherein the selectivity is 20% for batch mode and 41% for continuous mode.4. The process according to claim 1 , wherein the elevated pressure is in the range of 3 to 4 MPa for batch mode and 20 to 50 bar pressure for continuous mode.5. The process according to claim 4 , wherein the elevated pressure is in the range of 30-35 bar pressure for continuous mode.6. The process according to claim 1 , wherein the yield of THF is in the range of 20% for batch mode and 40% for continuous mode.7. The process according to claim 1 , wherein the temperature is 493 K for batch mode and in the range of 423 to 513 K for continuous mode.8. The process according to. claim 7 , wherein the temperature is in the range of 473 to 493 K for continuous mode.9. The process according to claim 1 , wherein the related ring hydrogenated products are selected from the group consisting of methyl tetrahydrofuran (MTHF) claim 1 , tetrahydrofurfuryl alcohol (THFAL) claim 1 , Methyl Furan claim 1 , and Pentanediol.10. The process according to claim 1 , wherein said catalyst is recyclable. The present ...

Prepn. of optically active 2-oxetanone derivs. - by hydrodechlorination of 4-(tri:, di: or mono:chloromethyl)-2-oxetanone(s) using tri: N-butyl tin hydride

The prepn. of optically active 2-oxoetanones of formula (I) comprises partial or complete dehalogenation of optically active 2-oxetanones of formula (II) in the presence of tri-n-butyl tin hydride under radical conditions. In the formula, R = H or Me R1 = CHCl2, CH2Cl or Me, provided that R and R1 are not both Me; R2 = CHCl3, CHCl2 or CH2Cl, provided that R2 contains at least on Cl atom more than R1. (S)- and (R)- 4-dichloromethyl-4-methyl -2-oxetanone (Ia) are new. The reaction is carried out in a hydrocarbon (esp. cyclohexane or benzene) or ester as solvent. The radical initiator is azobisisobutanonitrile or UV light. USE/ADVANTAGE - (I) are chiral building blocks which can be converted into a wide variety of prods. by hydrolysis or reaction with different reagents. These reactions are largely stereospecific; thus optically pure (I) give optically pure prods.. For example (I; R=H; R1=CH2Cl) can be hydrolytically ring opened to give 4-chloro-3-hydroxybutanoic acid which can be converted into carnitine using trimethylamine.

Synthesis of functionalized and unfunctionalized olefins via cross and ring-closing Metathesis

The invention is directed to the cross-metathesis and ring-closing metathesis reactions between geminal disubstituted olefins and terminal olefins, wherein the reaction employs a Ruthenium or Osmium metal carbene complex. Specifically, the invention relates to the synthesis of α-functionalized or unfunctionalized olefins via intermolecular cross-metathesis and intramolecular ring-closing metathesis using a ruthenium alkylidene complex. The catalysts preferably used in the invention are of the general formula wherein: M is ruthenium or osmium; X and X 1 are each independently an anionic ligand; L is a neutral electron donor ligand; and, R, R 1 R 6 , R 7 , R 8 , and R 9 are each independently hydrogen or a substituent selected from the group consisting of C 1 -C 20 alkyl, C 2 -C 20 alkenyl, C 2 -C 20 alkynyl, aryl, C 1 -C 20 carboxylate, C 1 -C 20 alkoxy, C 2 -C 20 alkenyloxy, C 2 -C 20 alkynyloxy, aryloxy, C 2 -C 20 alkoxycarbonyl, C 1 -C 20 alkylthio, C 1 -C 20 alkylsulfonyl and C 1 -C 20 alkylsulfinyl.

クロスメタセシスおよび閉環メタセシスによる、官能性および非官能性オレフィンの合成

本発明は、ルテニウムまたはオスミウムの金属カルベン錯体を使用する、一つの原子に１対の原子団が結合した（ジェミナル）の二置換オレフィンと末端オレフィンとの間のクロスメタセシスおよび閉環メタセシス反応に関する。詳細には、本発明は、ルテニウムアルキリデン錯体を使用する、分子間クロスメタセシスおよび分子内閉環メタセシスによる、α−官能性または非官能性オレフィンの合成に関する。本発明で使用される触媒は、好ましくは、一般式（Ｉ）または（ＩＩ）を有し、式中、Ｍはルテニウムまたはオスミウムであり、ＸとＸ １ は各々独立して陰イオン配位子であり；Ｌは中性の電子供与体配位子であり；Ｒ，Ｒ １ ，Ｒ ６ ，Ｒ ７ ，Ｒ ８ およびＲ ９ は、各々独立して水素またはＣ １ −Ｃ ２０ アルキル、Ｃ ２ −Ｃ ２０ アルケニル、Ｃ ２ −Ｃ ２０ アルキニル、アリル、Ｃ １ −Ｃ ２０ カルボキシレート、Ｃ １ −Ｃ ２０ アルコキシ、Ｃ ２ −Ｃ ２０ アルケニルオキシ、Ｃ ２ −Ｃ ２０ アルキニルオキシ、アリルオキシ、Ｃ ２ −Ｃ ２０ アルコキシカルボニル、Ｃ １ −Ｃ ２０ アルキルチオ、Ｃ １ −Ｃ ２０ アルキルスルホニルおよびＣ １ −Ｃ ２０ アルキルスルフィニルから選択される置換基である。 【化１９】

Proceso mejorado para la manufactura de tetrahidrofurano.

El proceso descrito se refiere a un proceso mejorado para manufacturar THF a partir de una mezcla de reacción que comprende BDO en la presencia de un catalizador ácido en un recipiente de reacción que comprende una zona de reacción de destilación, en donde el catalizador ácido se suspende en una región rica en vapor en la zona de reacción de destilación.

Catalytic coating for the hydrogenation of maleic anhydride and related compounds to give gamma-butyrolactone, tetrahydrofuran and derivatives thereof

The invention relates to a catalyst for the hydrogenation of C4 dicarboxylic acids and/or derivatives thereof, preferably maleic anhydride, in the gas phase, characterised in that said catalyst comprises 5 to 100 wt %, preferably 40 to 90 wt % copper oxide and 0 to 95 wt %, preferably 10 to 60 wt % of one or more metals, or compounds thereof, from the group comprising Al, Si, Zn, Pd, La, Ce, elements of groups III A to VIII A and of groups I A and II A as active mass and said mass is deposited on an inert support in the form of a thin layer.

Verfahren zur herstellung von alkoholen durch hydrierung von carbonylverbindungen

Ein Verfahren zur Herstellung von Alkoholen durch katalytische Hydrierung von Carbonylverbindungen mit Wasserstoff oder Wasserstoff enthaltenden Gasen in Gegenwart eines Hydrierkatalysators nach Raney, wobei der Katalysator in Form von Hohlkörpern eingesetzt wird. Als katalytisch aktive Bestandteile werden bevorzugt Nickel, Kobalt, Kupfer, Eisen, Platin, Palladium oder Ruthenium verwendet.

USE OF COATED CATALYSTS FOR THE HYDROGENATION OF MALEIC ANHYDROID TO GIVE TETRAHYDROFURAN AND GAMMA-BUTYROLACTONE.

TETRAHIDROFURANO Y GAMMA-BUTIROLACTONA SE PREPARAN PARTIENDO DE, AL MENOS, ANHIDRIDO MALEICO O ANHIDRIDO SUCINICO, MEDIANTE LA HIDROGENACION CATALITICAMENTE DE ANHIDRIDO MALEICO VAPOROSO O ANHIDRIDO SUCINICO VAPOROSO, EN PRESENCIA DE HIDROGENO, EN CONTACTO CON UN CATALIZADOR QUE COMPRENDE UN SOPORTE ESENCIALMENTE INERTE, AL MENOS PARCIALMENTE POROSO, QUE TIENE UNA SUPERFICIE EXTERIOR, Y UN MATERIAL OXIDO CATALITICAMENTE ACTIVO, REVISTIENDO SOBRE LA SUPERFICIE EXTERIOR DEL SOPORTE, QUE FUERTEMENTE SE ADHIERE AL SOPORTE, DONDE EL MATERIAL OXIDO CATALITICAMENTE ACTIVO COMPRENDE LOS OXIDOS MEZCLADOS DE COBRE, CINZ Y ALUMINIO. TETRAHIDROFURANO AND GAMMA-BUTIROLACTONA ARE PREPARED FROM, AT LEAST, MALEIC ANHYDRIDE OR SUCINIC ANHYDRIDE, THROUGH THE HYDROGENATION CATALYTICALLY OF MACHINE VAPOROSO, ENERGY PRESIDENT, VARIOUS LESS partially porous, having an outer surface and a oxide material catalytically active coating ON THE OUTER SURFACE OF THE SUPPORT THAT STRONGLY JOINS THE SUPPORT WHERE THE MATERIAL OXIDE catalytically active UNDERSTANDS oxides MIXED COPPER, ICZN and aluminum.

Conversion of tetrahydroxybutane to tetrahydrofuran

Catalytic coating to hydrogenate maleic anhydride and related compounds to obtain γ-butyrolactone, tetrahydrofuran and derivatives thereof

본 발명은 구리 옥시드 5 내지 100 중량％, 바람직하게는 40 내지 90 중량％ 및 Al, Si, Zn, Pd, La, Ce, IIIA족 내지 VIIIA족 및 IA족 내지 IIA족의 원소로 구성되는 군으로부터의 하나 이상의 금속, 또는 그의 화합물 0 내지 95 중량％, 바람직하게는 10 내지 60 중량％를 활성 조성물로서 포함하고, 상기 조성물은 불활성 지지체 상에 박층의 형태로 침착되는 것을 특징으로 하는, C 4 디카르복실산 및(또는) 그의 유도체, 바람직하게는 말레산 무수물의 기체 상에서의 수소첨가를 위한 촉매에 관한 것이다. The present invention comprises from 5 to 100% by weight of copper oxide, preferably from 40 to 90% by weight and an element of Al, Si, Zn, Pd, La, Ce, Groups IIIA to VIIIA and Groups IA to IIA C 4 , characterized in that it comprises 0 to 95%, preferably 10 to 60%, by weight of at least one metal, or compound thereof, as an active composition, said composition being deposited in the form of a thin layer on an inert support. A catalyst for the hydrogenation of dicarboxylic acids and / or derivatives thereof, preferably maleic anhydride, in the gas phase. 수소첨가 촉매, 지지체 물질, 촉매적 활성 물질 Hydrogenated Catalysts, Support Materials, Catalytically Active Materials

醚的制备方法

醚的制备方法，可选地，同时制备二醇和/或内酯，该方法由相应的有机原料在氢存在下进行反应，原料选自不饱和二羧酸和/或酐，不饱和二羧酸和/或酐的单酯，不饱和二羧酸和/或酐的二酯，不饱和内酯，以及上述两种或多种物质的混合物，包括以下步骤：(a)将含有至少一部分有机原料的物流导入预反应器区，该反应区含有催化剂，并在反应条件下运行，使所述原料与含氢气流接触，由此至少一部分碳碳双键被饱和；(b)在蒸发区，将至少一部分饱和原料蒸发到含氢气流中；(c)将含有被蒸发的至少部分饱和原料的含氢气流导入反应区，该反应区含有催化剂，并在反应条件下运行；(d)将产物流从反应区回收，所述产物流包含醚，可选地，还包含二醇和/或内酯；以及(e)将其余的含氢气流至少循环到预反应器区或蒸发区。

Preparation of 5-methylbutyrolactone

5-Methylbutyrolactone is prepared by a process in which a pentenoic ester of the formula I X--CO.sub.2 R (I), where X is CH 2 ═CH--CH 2 --CH 2 --, CH 3 --CH═CH--CH 2 -- or CH 3 --CH 2 --CH═CH-- and R is alkyl, cycloalkyl, aralkyl or aryl, or a mixture of these esters is reacted with water at from 50° to 350° C. in the presence or absence of a diluent a) over a zeolite and/or phosphate catalyst or b) in the presence of from 0.01 to 0.25 mole of a sulfonic acid, a Lewis acid and/or a non-oxidizing mineral acid per mole of pentenoic ester or over from 0.1 to 40% by weight, based on the pentenoic ester, of a strongly acidic ion exchanger as a catalyst in a first stage, or the pentenoic ester of the formula I, where X and R have the stated meanings, is hydrolyzed in a first stage with the aid of a strongly acidic ion exchanger as a catalyst to give the pentenoic acid of the formula I, where R is hydrogen, and the resulting pentenoic acid is subjected to cyclization in a second stage in the presence of from 0.005 to 0.1 mole of a sulfonic acid, a Lewis acid or a non-oxidizing mineral acid per mole of pentenoic acid or over from 0.1 to 20% by weight, based on the pentenoic acid, of a strongly acidic ion exchanger at from 50° to 350° C.

The method of obtaining-caprolactone

1,2,4- Trioxepanes as precursors for lactones

The present invention pertains to a novel process for the preparation of lactones by decomposition of a 1,2,4-trioxepane of formula (I) wherein, R is H or CH 3 , n is 1-14, Rx independently is any substituent on the ring structure, including substituents which form bi- or tricyclic structures, and m is 0-34.

How to prepare gamma-butyrolactone

본 발명은 2,5-디히드로푸란 또는 2,3-디히드로푸란 또는 그것들의 혼합물을 수소화 촉매상에서, 상승된 온도에서, 부가 수소의 존재 또는 부재하에, 및 물의 존재하에, 기체상으로 반응시키는 것을 특징으로 하는, 감마-부티로락톤의 제조 방법에 관한 것이다. The present invention is directed to reacting 2,5-dihydrofuran or 2,3-dihydrofuran or mixtures thereof in the gas phase on a hydrogenation catalyst, at elevated temperatures, in the presence or absence of additional hydrogen, and in the presence of water. It relates to a method for producing gamma-butyrolactone, characterized in that.

Bis-epsilon-caprolactones

1,2,4,-trioxepanes as precursors for lactones

The present invention pertains to a novel process for the preparation of lactones by decomposition of a 1,2,4-­trioxepane of formula (I) wherein, R is H or CH3, n is 1-14, Rx independently is any substituent on the ring structure, including substituents which form bi- or tricyclic structures, and m is 0-34.

Method for the distillative processing of tetrahydrofuran

본 발명은 극성 용매의 존재하에 테트라히드로푸란을 증류 정제하기 위한 방법을 제공한다. The present invention provides a method for distillative purification of tetrahydrofuran in the presence of a polar solvent. 테트라히드로푸란, 증류 정제, 극성 용매, 알카놀 Tetrahydrofuran, distillation tablets, polar solvents, alkanols

Ruthenium-optically active phosphine complex, process for producing the same, and process for producing optically active 4-methyl-2-oxetanone using the same

Treatment method and system for recycling tetrahydrofuran in solution discharged in parecoxib normal-phase workshop section

一种帕瑞昔布正相工段排放溶液回收四氢呋喃的处理方法及其系统。该处理系统包括：废液贮罐、提升泵、膜分离装置、冷凝回收装置、四氢呋喃收集罐、真空泵装置。废液贮罐与提升泵连接，提升泵通过管道与膜分离装置的液体入口连接，膜分离装置的液体出口与废液贮罐连接，膜分离装置的气体出口与冷凝回收装置连接，冷凝回收装置的液体出口与四氢呋喃收集罐连接，冷凝回收装置的气体出口与真空泵装置连接，真空泵装置与膜分离装置连接。本发明与传统技术相比，改变了帕瑞昔布正相工段废液的四氢呋喃回收的处理方式；无二次污染，无蒸馏釜残液产生，分离后四氢呋喃纯度高，直接回用至前端生产过程；整个过程在小于70℃的温度下进行，不会对溶液中的产品造成破坏；运行成本低。

The method of obtaining the derivative of indolo (2,3-a) quinolizina or its salts

Method for producing ketene dimer

Butyrolactone-preparation process

公开了一种制备通式Ⅰ的丁内酯的方法:其中取代基R 1 和R 2 是氢、烷基或羟烷基或任选带有惰性取代基的芳基和三烷基甲硅烷基,包括在提高的温度和压力下,在有过渡金属催化剂存在的条件下,使通式Ⅱ的炔与一氧化碳和氢气,或与一氧化碳和水反应:R 1 －C≡C－R 2 Ⅱ其中取代基的意义与上面相同。

Base Resin for Resist Material

하기 화학식 1로 표시되는 에스테르 화합물. 식중, R 1 은 수소 원자 또는 메틸기를 나타내고, R 2 는 탄소수 4 내지 20의 3급 알킬기를 나타내고, k는 0 또는 1이다. 본 발명의 에스테르 화합물을 중합함으로써 얻어지는 폴리머를 사용하여 조제한 레지스트 재료는 고에너지선에 감응하고 감도, 해상성, 에칭 내성이 우수하고, 전자선이나 원자외선에 의한 미세 가공에 유용하다. 특히 ArF 엑시머 레이저, KrF 엑시머 레이저의 노광 파장에서의 흡수가 작고, 또한 기판 밀착성이 우수하기 때문에 미세하고 또한 기판에 대하여 수직인 패턴을 용이하게 형성할 수 있으며 초 LSI 제조용의 미세 패턴 형성 재료로서 적합하다. 에스테르 화합물, 지환 구조, 옥시란 구조, 제조 방법

Preparation method of e-caprolactone

一种通过氧化环己酮制备ε－己内酯的方法，包括：将粗反应混合物送入第一蒸馏塔中；从第一蒸馏塔的塔顶蒸出包含低沸点组分的第一馏出物，该低沸点组分包括未反应的环己酮；从中间塔盘回收第一侧馏分，第一侧馏分中的未反应的环己酮的浓度比其在第一馏出物中的高；从第一蒸馏塔的塔底回收包含高沸点组分的第一塔底液体，该高沸点组分包括ε－己内酯；将第一侧馏分导入第二蒸馏塔中；从第二蒸馏塔的塔底回收包含未反应的环己酮的第二塔底液体；将第二塔底液体再循环至原料环己酮中；将第一塔底液体导入第三蒸馏塔中，以从第三蒸馏塔中得到包含ε－己内酯的第三馏出物。

Process for producing a lactone

하기 단계(1) 내지 (6): Steps (1) to (6) below: (1) 수소화 반응 대역으로부터 액체상을 회수하는 제1단계, (2) 첫번째 증류컬럼에서 액체상을 증류하여 첫번째 증류물 및 첫번째 잔류물을 수득하는 제2단계, (3) 첫번째 잔류물을 수소화 반응 대역으로 재순환 시키는 제3단계, (4) 두 번째 증류컬럼에서 첫번째 잔류물의 일부를 증류하여, 두 번째 증류물 및 두 번째 잔류물을 수득하는 제4단계, (5) 두 번째 증류물을 수소화 반응 대역 또는 첫번째 증류컬럼으로 재순환시키는 제5단계, (6) 첫번째 증류물로부터 락톤을 회수하는 제6단계 로 구성됨을 특징으로 하는, 루테늄 및 유기 포스핀으로 구성된 촉매의 존재하에 수소화 반응 대역으로 용매를 사용한 액체상 중에 디카르복실산, 디카르복실산 무수물 및/또는 디카르복실산 에스테르를 수소와 함께 반응시킴으로써 락톤을 제조하는 방법. (1) the first step of recovering the liquid phase from the hydrogenation zone, (2) the second step of distilling the liquid phase in the first distillation column to obtain the first distillate and the first residue, and (3) the first residue to the hydrogenation zone A third step of recycling to (4) a fourth step of distilling a portion of the first residue in a second distillation column to obtain a second distillate and a second residue, and (5) a hydrogenation reaction zone of the second distillate. Or a fifth step of recycling to the first distillation column, and (6) a sixth step of recovering lactone from the first distillate, using a solvent as the hydrogenation zone in the presence of a catalyst consisting of ruthenium and organic phosphine. A process for producing lactone by reacting dicarboxylic acid, dicarboxylic anhydride and / or dicarboxylic acid ester with hydrogen in the liquid phase.

Maleic anhydride hydrogenation changes into tetrahydrofuran (THF) and the used coated catalysts of gamma-butyrolactone

自马来酐或琥珀酐制备四氢呋喃和γ-丁内酯， 是在氢存在下将气相马来酐或气相琥珀酐与一催化 剂接触进行催化氢化。该催化剂包括一基本上是惰 性、至少有部分孔隙、具有外表面的载体和一有催化 活性的氧化物材料组成，该催化活性氧化物材料涂覆 在载体的外表面并牢固粘附于其上。催化活性氧化 物材料包括铜、锌和铝的氧化物混合物。

Ferroelectric liquid crystal device

내용 없음. No content.

Process for the simultaneous production of maleic anhydride and its hydrogenated derivatives

본 발명은 무수 말레산과 부탄-1,4-디올, γ-부티롤락톤 및 테트라하이드로퓨란에서 선택되는 C 4 화합물의 공동 제조에 관한 것으로, C 4 탄화수소 공급물의 부분 산화에 의해 무수 말레산, 물, 미전환 탄화수소 공급물 및 탄소 산화물을 포함하는 기상 반응 배출 스트림을 제조하여 무수 말레인산을 제공하는 것이다. 기상 반응 배출 스트림에 존재하는 무수 말레인산의 일부가 축합되어 미정제 무수 말레인산 스트림을 형성하고 잔량의 무수 말레인산을 함유하는 잔류 기상 스트림이 남게 된다. 또한 잔류 기상 스트림으로부터 유기 용매, 물 또는 수용액 상에서 무수 말레인산을 흡수한다. 이후, 무수 말레인산을 장입된 액상 흡수 매체로부터 회수한다. 상기 적어도 하나의 C 4 화합물은 무수 말레산, 말레산, 말레산디알킬, 이들의 2개 이상의 혼합물로 이루어진 C 4+ 공급물의 수소화에 의해 생산되는 것이다. 상기 방법은 기상 반응 배출 스트림이 단계(ⅲ) 전에 냉각되고, 인-흡수 물질의 보호상(gurad bed)이 단계(ⅲ) 전에 냉각된 기상 반응 배출 스트림의 경로에 위치하여 인-함유 물질이 스트림으로부터 제거되며, 단계(ⅲ)의 상기 미정제의 무수 말레산의 스트림 물질은 단계(ⅷ)의 C 4+ 수소화 공급물로 사용되거나 또는 단계(ⅷ)의 C 4+ 수소화 공급물을 제조하기 위해 사용되는 것을 특징으로 한다. The present invention relates to the co-production of a C 4 compound selected from maleic anhydride with butane-1,4-diol, γ-butyrolactone and tetrahydrofuran, wherein maleic anhydride, water by partial oxidation of a C 4 hydrocarbon feed And a gaseous reaction discharge stream comprising unconverted hydrocarbon feed and carbon oxides to provide maleic anhydride. Some of the maleic anhydride present in the gaseous reaction discharge stream is condensed to form a crude maleic anhydride stream and a residual gaseous stream containing the remaining amount of maleic anhydride is left. It also absorbs maleic anhydride in an organic solvent, water or aqueous solution from the residual gaseous stream. The maleic anhydride is then recovered from the charged liquid absorption medium. The at least one C 4 compound is one produced by hydrogenation of a C 4+ feed consisting of maleic anhydride, maleic acid, dialkyl maleate, a mixture of two or more thereof. The process is characterized in that the gaseous reaction discharge stream is cooled before the step, and a guard bed of the phosphorus-absorbing material is placed in the path of the cooled gaseous reaction discharge stream before the step, so that the phosphorus-containing material is streamed. From which the crude stream material of crude maleic anhydride in ...

Novel Ester Compounds Having Alicyclic and Oxirane Structures and Method for Preparing the Same

하기 화학식 1로 표시되는 에스테르 화합물. 식중, R 1 은 수소 원자 또는 메틸기를 나타내고, R 2 는 탄소수 4 내지 20의 3급 알킬기를 나타내고, k는 0 또는 1이다. 본 발명의 에스테르 화합물을 중합함으로써 얻어지는 폴리머를 사용하여 조제한 레지스트 재료는 고에너지선에 감응하고 감도, 해상성, 에칭 내성이 우수하고, 전자선이나 원자외선에 의한 미세 가공에 유용하다. 특히 ArF 엑시머 레이저, KrF 엑시머 레이저의 노광 파장에서의 흡수가 작고, 또한 기판 밀착성이 우수하기 때문에 미세하고 또한 기판에 대하여 수직인 패턴을 용이하게 형성할 수 있으며 초 LSI 제조용의 미세 패턴 형성 재료로서 적합하다.

Process for the production of ñò-butyrolactone

내용 없음. No content.

Process for preparation of diketene

Сущность изобретени : продукт - дике- тен (4-метилен-2-оксетан). Реагент 1: кетен. Услови  реакции: ингибитор - диоксид серы в концентрации 30-5700 част/мил. 3 табл

Manufacture of lactone

Method for producing gamma-butyrolactone and tetrahydrofuran

(57)【要約】 n-ブタンの変換工程から回収した無水マレイン酸の水素化によるテトラヒドロフラン及びガンマブチロラクトンの製造方法。 以下の工程より構成される方法を提供する。A) n-ブタンを接触蒸気相酸化により無水マレイン酸へ変換する工程、B) ブタン酸化により生ずる排出ガスからガンマブチロラクトン中での選択的吸収によって無水マレイン酸を回収する工程、C) ガス作用下及び／または真空条件下で除去装置中の無水マレイン酸−ガンマブチロラクトン混合物から水分を除去して水分及びマレイン酸の含量が最小となる無水マレイン酸−ガンマブチロラクトン混合物を生成する工程、D) 無水マレイン酸からの排出ガス中に含まれるガンマブチロラクトンを水中で吸収して回収する工程、E) 回収したガンマブチロラクトンを脱水してそれを無水マレイン酸吸収装置へリサイクルする工程、F) 脱水した無水マレイン酸−ガンマブチロラクトン混合物を1または2以上の触媒を用いてテトラヒドロフラン及びガンマブチロラクトンの生成に有利な条件下で水素化する工程、G) 得られた水素化混合物からテトラヒドロフラン、ガンマブチロラクトン及び副生物を蒸留により分離する工程、及びH) ガンマブチロラクトン濃厚液流を無水マレイン酸吸収装置へリサイクルする工程。

Odorable composition

Preparation method of gamma butyrolactone using maleic anhydride

본 발명은 무수말레인산을 원료로 한 감마 부티로락톤 제조방법이다. The present invention is a method for producing gamma butyrolactone using maleic anhydride as a raw material. 그 구성은 표면적이 큰 실리카(silica)에 담지된 팔라듐(palladium)과 몰리브덴(molybdenum) 그리고 니켈(nickel)로 구성된 귀금속 촉매를 이용하여 액상에서 MAN(말레산 무수물(maleic anhydride)) 또는 SA(숙신산 무수물(succinic anhydride))를 GBL(감마 부티로락톤(gamma Butyrolactone))로 전환하는 개선된 수소화 촉매반응 공정으로 되어 있다. Its composition consists of MAN (maleic anhydride) or SA (succinic acid) in the liquid phase using a noble metal catalyst composed of palladium, molybdenum and nickel supported on silica with a large surface area. An improved hydrogenation catalysis process converts anhydrous (succinic anhydride) into GBL (gamma Butyrolactone). 이때의 수소화 촉매반응은 수소압력 50∼150 kg/cm 2 으로 150∼350℃의 온도범위 하에서 수행하였다. At this time, the hydrogenation catalysis was performed under a temperature range of 150 to 350 ° C. at a hydrogen pressure of 50 to 150 kg / cm 2 .

γ-BUTYROLACTONE PRODUCTION PROCESS

Описывается способ получения γ -бутиролактона, согласно которому осуществляют превращение 2,5-дигидрофурана или 2,3-дигидрофурана, или их смеси в газовой фазе в присутствии воды и в присутствии или в отсутствии добавляемого водорода при повышенных температурах на катализаторе гидрирования. Технический результат - разработка экономического способа получения целевого продукта. 9 з.п.ф-лы. ГбузЗ$ гс ПЧ Го (19) РОССИЙСКОЕ АГЕНТСТВО ПО ПАТЕНТАМ И ТОВАРНЫМ ЗНАКАМ ВИ ”2 138 491 ' 50 МК С 070 307/32 13) СЛ 12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ РОССИЙСКОЙ ФЕДЕРАЦИИ (21), (22) Заявка: 96113048/04, 17.06.1996 (30) Приоритет: 18.11.1993 ОЕ Р 4339269.5 (46) Дата публикации: 27.09.1999 (56) Ссылки: С. Рапсае! е а!. "Руп4тит Стогосйготае т {Ле Огдапс эзупе$15: А Сопуетейт ОхааНоп о? Епо|-Еега фо ЕЗег$ апа Гасюпе$", {гапедгоп ей., ТЭ7Р, 39, 3483-3484. гамма-лактоны -М.: НИИТЭХИМ, 1989. ($ 4968818 А, 06.11.90. ЕР 0276012 АД, 27.02.88. (85) Дата перевода заявки РСТ на национальную фазу: 18.06.96 (86) Заявка РСТ: ЕР 94/03683 (17.06.96) (87) Публикация РСТ: М/О 95/14010 (26.05.95) (98) Адрес для переписки: 103064, Москва, ул.Казакова 16, НИИР-Канцелярия, Патентные поверенные Квашнин, Сапельников и Партнеры (71) Заявитель: БАСФ АГ (О0Е) (72) Изобретатель: Рольф Пинкос (0Е), Рольф Фишер (0Е) (73) Патентообладатель: БАСФ АГ (0Е) (54) СПОСОБ ПОЛУЧЕНИЯ у-БУТИРОЛАКТОНА (57) Реферат: Описывается способ получения у -бутиролактона, согласно которому осуществляют — превращение 2,5-дигидрофурана или 2,3-дигидрофурана, или их смеси в газовой фазе в присутствии воды и в присутствии или в отсутствии добавляемого водорода при повышенных температурах на катализаторе гидрирования. Технический результат - разработка экономического способа получения целевого продукта. 9 з.п.ф-лы. 2138491 С1 КО ГбузЗ$ гс ПЧ Го (19) КУЗЗАМ АСЕМСУ ГОК РАТЕМТ$ АМО ТКАОЕМАКК$ 12) АВЗТКАСТ ОЕ 1МУЕМТОМ 13) ВИ “” 2438 491 ^^ С1 (51) п. С1.8 С 070 307/32 (21), (22) АррИсаНоп: 96113048/04, 17.06.1996 (30) Рпогйу: 18.11.1993 ОЕ Р ...

A kind of method preparing anhydrous level oxolane

本发明公开了一种无水级四氢呋喃试剂的制备方法，该制备方法包括如下步骤：首先通过格氏反应将工业级四氢呋喃中的微量醇、羰基化合物和过氧化物转化为高沸点或低挥发性化合物，再进一步采用精馏得到无水级四氢呋喃，本发明的优点为回收率高、制备方法简单、高效，适用于高纯试剂的生产。

Patent SU392623A3

Method of gamma-butyrolactone synthesis

According to this process, gamma-butyrolactone is produced by liquid phase catalytic hydrogenation of maleic anhydride with hydrogen at elevated temperature and under pressure, in the presence of a catalyst containing nickel and palladium deposited on a support. …<??>When the support material chosen is a support based on silica exhibiting a very high specific surface whose value can range from 50 m<2>/g, preferably from approximately 100 m<2>/g up to 800 m<2> and more, very high degrees of conversion are obtained, of the order of 90 to 98 mol%, together with excellent selectivities for gamma-butyrolactone, of 95 to 97 mol%.

A kind of process for purification of water-containing tetrahydrofuran

本发明是涉及一种含水四氢呋喃的精制方法。该技术方案采用四氢呋喃原料液汽化和富含水的四氢呋喃再生解析凝液脱水回收为一体的多功能四氢呋喃脱水塔、填料与板式塔复合精馏塔、变压吸附、汽提吸附和能量多级多效利用等技术，通过四氢呋喃精馏脱水及吸附脱水操作单元，实现了以含水浓度接近共沸组成的四氢呋喃原料液生产低含水量的四氢呋喃产品的生产过程，生产流程简捷，能耗低，四氢呋喃精制脱水操作过程本质安全，有效地解决了接近四氢呋喃与水共沸组成的含水四氢呋喃原料液进一步精制脱除共沸水操作，不能采用常规精馏工艺，而萃取精馏工艺存在工艺复杂，蒸汽消耗，设备投资大和操作成本高等问题，具有较强的市场推广前景。

A kind of method by coupling rectification purification of tetrahydrofuran

本发明涉及一种通过耦合精馏提纯四氢呋喃的方法，将低浓度四氢呋喃加入预处理塔，经加热汽化后上升至塔顶，冷凝为液体后，一部分回流入预处理塔，一部分送至共沸物中间罐；将稳定剂、共沸物中间罐内液体加入加压塔，落入塔釜的物料加热汽化，经耦合再沸器冷凝为液体，一部分液体回流入加压塔，另一部分进入常压脱水塔，加热汽化上升至常压脱水塔塔顶后，冷凝为液体，一部分液体返回常压脱水塔，另一部分送至共沸物中间罐。该方法的优点：得到的产品所含四氢呋喃的质量分数达99.98％，含水量小于200ppm；通过双效耦合，节省能耗，降低成本；加入稳定剂、还原剂，解决了四氢呋喃容易形成过氧化物的问题，大大降低装置的危险性。

Process for the preparation of macrocyclic esters

Verfahren zur Herstellung makrocyclischer Esterverbindungen der Formel worin x und y in Summe eine Zahl von mindestens 10 und höchstens 13 ergeben; A eine Methylengruppe oder ein Heteroatom wie Sauerstoff oder Schwefel bedeuten kann; B eine Methylengruppe oder eine Carbonylgruppe bedeuten kann oder A und B zusammengenommen eine Kohlenstoffdoppelbindung bedeuten können; durch Kondensation von difunktionellen Verbindungen der Formel worin x und y in Summe eine Zahl von mindestens 10 und höchstens 13 ergeben; A eine Methylengruppe oder ein Heteroatom wie Sauerstoff oder Schwefel bedeuten kann; B eine Methylengruppe bedeuten kann oder A und B zusammengenommen eine Kohlenstoffdoppelbindung bedeuten können; R 1 ein Wasserstoffatom, Methyl oder Ethyl bedeuten kann; oder der Formel worin x und y in Summe eine Zahl von mindestens 10 und höchstens 13 ergeben; R 1 ein Wasserstoffatom, Methyl oder Ethyl bedeuten kann; ... Process for the preparation of macrocyclic ester compounds of the formula wherein x and y add up to a number of at least 10 and at most 13; A can represent a methylene group or a hetero atom such as oxygen or sulfur; B may represent a methylene group or a carbonyl group or A and B taken together can represent a carbon double bond; by condensation of difunctional compounds of the formula wherein x and y add up to a number of at least 10 and at most 13; A can represent a methylene group or a hetero atom such as oxygen or sulfur; B may represent a methylene group or A and B taken together may represent a carbon double bond; R 1 can represent a hydrogen atom, methyl or ethyl; or the formula wherein x and y add up to a number of at least 10 and at most 13; R 1 can represent a hydrogen atom, methyl or ethyl; ...

Composition for the prevention and treatment of inflammatory diseases comprising the penicillinolide A isolated from marine fungi

본 발명은 페니실리움 속( Penicillium sp.) SF-5292 균주로부터 분리한 항염활성을 갖는 신규한 페니실리놀라이드(Penicillinolide) A 화합물 및 이의 용도에 관한 것으로서, 본 발명의 해양 진균에서 분리한 페니실리놀라이드 A는 염증과 관련된 사이토카인인 IL-1β, TNF-α, IL-6, NO 및 PGE 2 의 생성 및 활성화를 효과적으로 억제하고, 염증을 직접적으로 유도할 수 있는 NO의 분비를 효과적으로 억제하며, 염증 유도 단백질 발현 억제 물질의 핵 내로의 이동을 억제하고, 산화적 스트레스로 인한 손상으로부터의 세포보호효과를 나타내는 효소로 알려진 HO-1의 발현 및 활성을 증가시키며, 천연물 유래 물질로 세포 독성도 낮아 안전성 및 부작용 관련 문제가 발생될 가능성도 낮으므로, 본 발명의 화합물은 염증성 질환 예방 또는 치료를 위한 조성물로 유용하게 사용될 수 있다. The present invention relates to a pharmaceutical composition comprising Penicillium The present invention relates to a novel penicillinolide A compound having anti-inflammatory activity isolated from a strain SF-5292 and its use, wherein the penicillinolide A isolated from marine fungi of the present invention is a compound of the formula Cain of IL-1β, TNF-α, IL-6, effectively inhibited the generation and activation of NO and PGE 2, and suppresses the NO release of which can lead to inflammation directly effectively, the inflammation induced protein expression inhibitory substance It inhibits migration into the nucleus, increases the expression and activity of HO-1, an enzyme known to exhibit cytoprotective effects from oxidative stress, and has low cytotoxicity due to natural products, resulting in safety and adverse side effects , The compounds of the present invention can be usefully used as a composition for the prevention or treatment of inflammatory diseases.

Process for preparing optically active 4-methyl-2-oxetanone

A process for preparing optically active 4-methyl-2-oxetanone which comprises asymmetrically hydrogenating 4-methylene-2-oxetanone in the presence of a ruthenium-optically active phosphine complex. Optically active 4-methyl-2-oxetanone can easily and economically be obtained at high optical purity.

Method for producing optically active 4-methyl-2-oxetanone

Processes for the manufacture of lactones

PREPARATION OF RESORCINOLS FROM D-CETOCARBOXYLIC ACIDS OR THEIR LACTONS

Simultaneous production of lactones and aromatic carboxylic acids

Process for the manufacture of alkyl ketene dimer

METHOD FOR REPRESENTING HIGH PURITY TETRAHYDROFURANE.

Method of synthesis of gamma-butyrolactone

Process for stabilizing lactones

Lactones are stabilized, particularly against discoloration, by mixing the lactone with oxygen, an oxidizing agent or an acid which is less volatile than the lactone and subjecting the mixture to distillation.

Benzocycloalkane derivatives and pharmaceutical compositions

Patent FR2351080B1

A process for asymmetrically hydrogenating through the use of microorganisms a double bond connected to tertiary carbon atom in an olefinic aliphatic compound to produce a tertiary, optically active aliphatic compound useful as an intermediate for optically active Vitamins E and K.

Process for preparing epsilon-caprolactones

Process for the continuous production of delta-valerolactone

Patent FR2197873B1

Patent FR2297851B1

Tricycloalkylidene peroxides - from 1-hydroxy-1'-hydro peroxydicyclohexyl peroxide or 1, 1'-dihydroperoxydicycloalkyl peroxi

Tricycloalkylidene peroxides are prepd. by reacting 1-hydroxy-11-hydroperoxydicyclohexyl peroxide or a 1,11-dihydroperoxydicyloalkyl peroxide with a cyclic ketone in an organic solvent contg. a strong acid catalyst. The rings may carry substituents. Dicyclohexylidene-2-methylcyclohexylidene peroxide, dicyclohexylidene octylidene peroxide, dicyclohexylidene cyclododecylidene peroxide, dicyclohexylidene-3-methyl-5-methoxycyclohexylidene peroxide, dicyclododecylidene cycloheptylidene peroxide and dicyclododecylidene cyclopentylidene peroxide are claimed. The peroxides are intermediates for macrocyclic products. They can also be used to crosslink polymers and as polymerisation initiators. They have antiparasitic, esp. antimalarial, activity. Solid ketones can be used. New peroxides can be obtained in high yield. The peroxide soln. obtained can be used directly for the conversion to macrocyclic cpds.

Patent FR2519985B1

New antifungal-6- alkyl-delta-lactone cpds.

6-Alkyl- delta -lactones of formula (I), in enantiomeric or racemic form, are new: R = -(CH2)n-CH3; n = 4-19 (pref. 5-11). Also new are (I) producing trichoderma strains, (II) having plant growth and germination stimulating activity and antifungal activity. Methods for selecting strains (II) are claimed; see 'Microorganism Selection' below.

Patent FR1604718A

Conversion of Tetrahydroxybutane to Tetrahydrofuran

본 발명에는, 지지된 레늄 촉매 및 산의 존재 하에서 테트라히드록시부탄을 수소 첨가시켜 테트라히드로푸란 및 그의 불포화 전구체를 형성하는 방법이 개시되어 있다. 테트라히드록시부탄, 테트라히드로푸란, 전구체, 레늄 촉매, 수소 첨가

Process for preparing chrysanthemum acid

Patent FR2000453A1

Macrocyclen

The invention is concerned with odorant compositions which contain macrocycles, namely 15- to 17-membered compounds of the formula (see fig. I) wherein the dotted line signifies an optional additional bond, X and Y stand for methylene or C2-12-polymethylene, optionally substituted with an additional methyl group, and A signifies hydrogen or methyl in the case of the unsaturated compound and methyl in the case of the saturated compounds, with the proviso that the unsaturated compounds are present to more than 80% in the cis form when A signifies hydrogen and are present to more than 50% in the cis form when A signifies methyl, with the exception of Z-oxacyclopentadec-6-en-2-one (15-membered ring), Z-oxacyclohepadec-8-en-2-one (17-membered ring) and Z-oxacycloheptadec-11-en-2-one (17-membered ring), a process for the manufacture of the compounds of formula I and the use of the compounds of formula I as odorants.

Patent FR2066528A5

PERFUME MIXTURES CONTAINING S-VALEROLACTONE

Mélanges de parfums. Ils contiennent comme constituant odoriférant une gamma , gamma -dialkyl sigma -lactone répondant à la formule : Mixtures of perfumes. They contain as an odoriferous constituent a gamma, gamma -dialkyl sigma -lactone corresponding to the formula:

Improvements in the preparation of lactones

PROCESS FOR THE PRODUCTION OF HETERO-MACROCYCLIC COMPOUNDS

L'invention concerne un procédé de production continu ou semi-continu de composés hétéro-macrocycliques comprenant des lactones et des esters cycliques. Le procédé comprend la dépolymérisation catalysée d'un polyester linéaire à une température élevée et sous pression réduite en présence d'une quantité spécifiée de monocarboxylates, tout en fournissant un brassage de haut en bas dans pratiquement tout le volume de la masse réactionnelle. Application à la production de composés hétérocycliques utilises comme agents parfumants. The invention relates to a process for the continuous or semi-continuous production of hetero-macrocyclic compounds comprising lactones and cyclic esters. The process comprises the catalyzed depolymerization of a linear polyester at elevated temperature and under reduced pressure in the presence of a specified amount of monocarboxylates, while providing top-to-bottom mixing throughout substantially the entire volume of the reaction mass. Application to the production of heterocyclic compounds used as perfuming agents.

Patent FR2415108B1

New 4-alkyl-gamma-lactone derivatives that stimulate plant growth and defense and have antifungal activity against pathogenic fungi

4-Alkyl-gamma-lactones (I) are new. 4-Alkyl-gamma-lactones of formula (I) are new: R1, R4 = H, alkyl, alkenyl, aralkyl or aralkenyl, provided that one is (CH2)nCH3; n = 0-19; R2, R3, R5, R6 = H, alkyl, alkenyl, aralkyl or aralkenyl. An Independent claim is also included for (I)-producing Trichoderma strains.

Patent FR2500453B1

PROCESS FOR THE PREPARATION OF A LOWER ALKYL DIESTER OF BRASSYLIC ACID

L'INVENTION CONCERNE UN NOUVEAU PROCEDE DE PREPARATION D'UN DIESTER D'ALKYLE INFERIEUR DE L'ACIDE BRASSYLIQUE DE FORMULE GENERALE: (CF DESSIN DANS BOPI) DANS LAQUELLE R EST UN GROUPE ALKYLE INFERIEUR. SELON L'INVENTION, ON FAIT REAGIR UN PERACIDE AVEC LA 2,2-METHYLENEBISCYCLOHEXANONE DANS UN SOLVANT ORGANIQUE HALOGENE EN PRESENCE D'UN CARBONATE ALCALIN POUR FORMER LE 6,6-METHYLENEBIS-(6-HEXANOLIDE) ET ON EFFECTUE L'HYDROCRAQUAGE DUDIT HEXANOLIDE DANS UN ALCOOL DE FORMULE:ROHDANS LAQUELLE R EST TEL QUE DEFINI CI-DESSUS, EN PRESENCE D'UN CATALYSEUR METALLIQUE ET D'UN CATALYSEUR ACIDE. THE INVENTION CONCERNS A NEW PROCESS FOR PREPARING A LOWER ALKYL DIESTER OF BRASSYLIC ACID OF GENERAL FORMULA: (CF DRAWING IN BOPI) IN WHICH R IS A LOWER ALKYL GROUP. ACCORDING TO THE INVENTION, A PERACID IS REACTED WITH 2,2-METHYLENEBISCYCLOHEXANONE IN A HALOGENIC ORGANIC SOLVENT IN THE PRESENCE OF AN ALKALINE CARBONATE TO FORM 6,6-METHYLENEBIS- (6-HEXANOLIDE) AND THE HYDROCRACKING PERFORMED. HEXANOLIDE IN AN ALCOHOL OF FORMULA: ROHD IN WHICH R IS AS DEFINED ABOVE, IN THE PRESENCE OF A METAL CATALYST AND AN ACID CATALYST.

Process for substituting the alpha position of gamma-lactones

Process for preparing epsiloncaprolactone

Process for preparing epsilon-caprolactone

Indicator device

Lactone stabilization process

4-Biphenyl-4-hydroxy-crotonic acid lactone - useful as an anti-inflammatory agent

Title lactones have the formula (I):- (where X is h or halogen). Cpds. (I) are useful as anti-inflammatory agents pref. administered in daily dose of 150-600 mg.

Acid accelerated hydrocarboxylation

New process for preparing chrysanthemic acid

Patent FR2110782A5

Patent FR2385394B1

New process for preparing pyrocine

PRODUCTION OF ALPHA PYRONS

NEW ETHERS WHOSE ORGANIC REMAINS CONTAIN CHIRAL ATOMS, THEIR PROCESS FOR PREPARATION AND THEIR APPLICATION TO THE DOUBLING OF ALCOHOLS, PHENOLS OR CERTAIN COMPOUNDS OF LACTONIC STRUCTURE

Composés de formule :

Carbonylation of epoxides

The invention relates a process for the carbonylation of epoxides by reaction with carbon monoxide at elevated pressure and temperature in the presence of a catalyst system comprising a source o.f cobalt and a hydroxy substituted pyridine compound, whereby .beta.-propiolactones and/or derivatives thereof, such as .beta.-propiolactone polymers, .beta.-hydroxy carboxylic acids and esters, and .beta.-alkoxy carboxylic acids and esters, are produced.