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Небесная энциклопедия

Космические корабли и станции, автоматические КА и методы их проектирования, бортовые комплексы управления, системы и средства жизнеобеспечения, особенности технологии производства ракетно-космических систем

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Мониторинг СМИ

Мониторинг СМИ и социальных сетей. Сканирование интернета, новостных сайтов, специализированных контентных площадок на базе мессенджеров. Гибкие настройки фильтров и первоначальных источников.

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Форма поиска

Поддерживает ввод нескольких поисковых фраз (по одной на строку). При поиске обеспечивает поддержку морфологии русского и английского языка
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Применить Всего найдено 2333. Отображено 100.
12-07-2012 дата публикации

Image processing method, and image processor

Номер: US20120176463A1
Принадлежит: Ricoh Co Ltd

The present invention provides an image processing method which includes at least any one of image recording and image erasing, wherein a light irradiation intensity at a center position of the laser beam irradiated in the image recording is controlled; in the image recording, a first auxiliary line extended by a predetermined distance from a start point of each of image lines constituting an image in the opposite direction from the scanning direction and a second auxiliary line extended by a predetermined distance from an end point of each of the image lines in the scanning direction are prepared, and when the first and second auxiliary lines including an image line are continuously scanned, the image line is scanned with irradiating the laser beam, and the first and the second auxiliary lines are scanned without irradiating the laser beam to thereby record the image.

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21-03-2013 дата публикации

PROCESS FOR PREPARING EXTRA PURE 2, 6-DIISOPROPYL PHENOL

Номер: US20130072573A1
Принадлежит: HARMAN FINOCHEM LIMITED

Disclosed herein is a process for the preparation of highly pure 2,6-diisopropyl phenol (Formula I), which comprises reacting p-hydroxy benzoic acid (Formula II) with an alkylating agent in presence of aq. mineral acid followed by basilication and subsequent washings to yield 4-hydroxy-3,5-diisopropylbenzoic acid (Formula III) free of dimer impurity, 4, 4′-oxy-dibenzoic acid of Formula IV, ether impurity 3,5-di(propan-2-yl)-4-(propan-2-yloxy)benzoic acid of Formula V and the monoalkylated impurity 4-hydroxy-3-(propan-2-yl) benzoic acid of Formula VI; and decarboxylating 4-hydroxy-3,5-diisopropylbenzoic acid (Formula III) in presence of high boiling solvent and sodium hydroxide as a catalyst at high temperature to yield 2,6-diisopropyl phenol substantially free of ether impurity 1,3-di(propan-2-yl)-2-(propan-2-yloxy)benzene of Formula VII and monoalkylated phenol impurity 2-(propan-2-yl) phenol of Formula VIII. Propofol prepared by the process of the present invention is suitable for pharmaceutical use. 16-. (canceled)8) The process of claim 7 , wherein step (b) comprises performing at least two steps selected from the group consisting of:i) washing said crude 4-hydroxy-3,5-diisopropylbenzoic acid with toluene at a basic pH to remove 3,5-di(propan-2-yl)-4-(propan-2-yloxy)benzoic acid;ii) washing said crude 4-hydroxy-3,5-diisopropylbenzoic acid with hot water to remove 4,4′-oxydibenzoic acid; andiii) removing 4-hydroxy-3-(propan-2-yl) benzoic acid from said crude 4-hydroxy-3,5-diisopropylbenzoic acid by either:washing said crude 4-hydroxy-3,5-diisopropylbenzoic acid with a mixture of methanol and water, orrecrystallizing said crude 4-hydroxy-3,5-diisopropylbenzoic acid from a mixture of methanol and water.9) The process of claim 7 , wherein step (b) comprises sequentially:i) washing said crude 4-hydroxy-3,5-diisopropylbenzoic acid with toluene at a basic pH to remove 3,5-di(propan-2-yl)-4-(propan-2-yloxy)benzoic acid;ii) washing said crude 4-hydroxy-3,5- ...

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20-06-2013 дата публикации

REVERSIBLE THERMOSENSITIVE RECORDING MEDIUM AND REVERSIBLE THERMOSENSITIVE RECORDING MEMBER

Номер: US20130157847A1
Принадлежит:

A reversible thermosensitive recording medium including a support, a reversible thermosensitive recording layer provided on the support and an antistatic layer, wherein the antistatic layer is provided on at least one of the reversible thermosensitive recording layer and a surface of the support opposite to the surface thereof on which the reversible thermosensitive recording layer is provided, wherein the antistatic layer contains spherical fillers and a curable conductive polymer, and wherein the spherical fillers satisfy the following Expression (1): 1. A reversible thermosensitive recording medium comprising:a support,a reversible thermosensitive recording layer provided on the support andan antistatic layer,wherein the antistatic layer is provided on at least one of the reversible thermosensitive recording layer and a surface of the support opposite to the surface thereof on which the reversible thermosensitive recording layer is provided,wherein the antistatic layer contains spherical fillers and a curable conductive polymer, and {'br': None, '4≦average particle diameter of the spherical fillers/thickness of the antistatic layer≦6\u2003\u2003Expression (1)'}, 'wherein the spherical fillers satisfy the following Expression (1)2. The reversible thermosensitive recording medium according to claim 1 , wherein a surface of the antistatic layer is covered with the spherical fillers at a coverage of 2% to 10%.3. The reversible thermosensitive recording medium according to claim 1 , wherein the average particle diameter of the spherical fillers is 10 μm to 20 μm.4. The reversible thermosensitive recording medium according claim 1 , wherein the thickness of the antistatic layer is 1 μm to 5 μm.5. The reversible thermosensitive recording medium according to claim 1 , wherein the antistatic layer has a surface resistance of 1×10Ω/sq. or lower.6. The reversible thermosensitive recording medium according to claim 1 , wherein the curable conductive polymer is a UV-curable ...

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08-08-2013 дата публикации

YIELD-EFFICIENT PROCESS FOR THE PRODUCTION OF HIGHLY PURE 2-METHYL-1, 4-NAPHTHOQUINONE AND ITS DERIVATIVES

Номер: US20130204019A1
Принадлежит:

The present invention discloses a process for the production of 2-methyl-1,4-naphthoquinone and its bisulfite adducts, comprising the following steps: a) oxidizing 2-methyl-naphthalene (2-MNA) to achieve an organic phase containing 2-methyl-naphthoquinone (2-MNQ) and 6-methyl-naphthoquinone (6-MNQ); b) subjecting said organic phase to treatment with an aqueous solution of a bisulfite salt to extract preferentially the 6-MNQ isomer from the organic phase; c) separating said organic phase from the aqueous phase; d) subjecting the organic phase of process step c) to a second bisulfitation step with an aqueous solution of a bisulfite salt, resulting in an organic phase containing 2-MNA and trace amounts of 2-MNQ and an aqueous phase containing 2-MSB and trace amounts of 6-MSB; e) optionally removing interfering bisulfite ions from the aqueous phase of process step c); f) raising the pH of the aqueous phase from step c) or e) to higher than 8.5 in the presence of a solvent resulting in an organic phase containing 2-MNQ; g) combining the organic phase from step f) with the organic phase being treated in the process step d); h) recycling the organic phase from step d) back to step a) to be used as solvent for the oxidation reaction of 2-MNA. 1. A process for the production of 2-methyl-1 ,4-naphthoquinone and its bisulfite adducts , comprising the following steps:a) oxidizing 2-methyl-naphthalene (2-MNA) to achieve an organic phase containing 2-methyl-naphthoquinone (2-MNQ) and 6-methyl-naphthoquinone (6-MNQ);b) subjecting said organic phase to treatment with an aqueous solution of a bisulfite salt to extract preferentially the 6-MNQ isomer from the organic phase;c) separating said organic phase from the aqueous phase;d) subjecting the organic phase of process step c) to a second bisulfitation step with an aqueous solution of a bisulfite salt, resulting in an organic phase containing 2-MNA and trace amounts of 2-MNQ and an aqueous phase containing 2-MSB and trace amounts of ...

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19-09-2013 дата публикации

PROCESS FOR THE OXIDATION OF HYDROCARBONS WITH THE USE OF IRIDIUM METAL CATALYST COMPLEXES

Номер: US20130245324A1
Принадлежит:

Provided is a process for effectively and efficiently oxidizing alkyl-containing molecules with the use of an oxygen-containing gas. An iridium metal catalyst complex with the iridium being coordinated with the nitrogen atoms of a benzimidazolyl-containing ligand is used as the catalyst. The process generates alcohols, ketones and aldehydes directly from alkyl-containing molecules and/or aromatic molecules. 1. A process for oxidizing alkanes and/or aromatics , which comprises contacting the alkanes and/or aromatics with oxygen in the presence of an iridium catalyst complex comprising iridium complexed with a benzimidazolyl-containing ligand.2. The process of claim 1 , wherein the complex is of the formula LMX(X′) claim 1 , where n=0 claim 1 , 1 or 2;{'sub': 1', '12', '1', '12', '3', '12', '3', '12', '6', '14', '7', '17, 'X and X′ are independently selected from the group consisting of halides, hydride, triflate, acetates, borates, Cthrough Calky, Cthrough Calkoxy, Cthrough Ccycloalkyl, Cthrough Ccycloalkoxy, Cthrough Caryl, Cthrough Caralkyl and olefins;'}M is iridium; andL is a benzimidazolyl-containing ligand.4. The process of claim 2 , wherein the benzimidazolyl-containing ligand is 2 claim 2 ,2′-(1 claim 2 ,3-phenylene)bis(1-propylbenzimidazol-2-yl).5. The process of claim 1 , wherein the iridium is coordinated with the nitrogen atoms in the benzimidazolyl-containing ligand to form an NCN pincer ligand complex.6. The process of claim 1 , wherein the iridium catalyst complex is used in combination with a co-catalyst.7. The process of claim 1 , wherein the process comprises oxidizing an alkane.8. The process of claim 7 , wherein the alkane is a C-Calkane.9. The process of claim 8 , wherein the alkane is a straight chain alkane.10. The process of claim 8 , wherein the alkane is a branched chain alkane.11. The process of claim 7 , wherein the alkane is a cycloalkane.12. The process of claim 1 , wherein the process comprises oxidizing an aromatic compound.13. The ...

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10-10-2013 дата публикации

PROCESS FOR THE PREPARATION OF ATOVAQUONE

Номер: US20130267717A1
Принадлежит: Glaxo Group Limited

Disclosed herein is novel process for preparation of atovaquone, which process includes reacting 1H-2-benzopyran-1,4(3H)-dione with 4-(4-chlorophenyl)cyclohexanecarbaldehyde. The invention further discloses novel intermediates useful in the preparation of atovaquone. 6. A process as claimed in wherein the reaction proceeds in the presence of a nucleophile/base.7. A process as claimed in wherein the nucleophile/base is sodium methoxide (NaOMe).8. A process as claimed in wherein the reaction proceeds in the presence of a catalyst or a base.9. A process as claimed in wherein the catalyst or base is morpholine.10. A process as claimed in wherein the catalyst or base is isobutylamine.11. A process as claimed in wherein the hydrogenating agent is Pd/C and dry activated carbon.15. (canceled) The present invention relates to a new process for the preparation of atovaquone. In particular, the present invention relates to novel intermediates useful in the preparation of atovaquone.Atovaquone, 2-[trans-4-(4-chlorophenyl)cyclohexyl]-3-hydroxy-1,4-naphthoquinone (compound of formula (I))is a useful medicine for the treatment and prophylaxis of infections. Atovaquone is potently active (in animals and in vitro) against , and tachyzoite and cyst forms of . Due to its inhibitory effect in sensitive parasites, atovaquone can act by selectively affecting mitochondrial electron transport and parallel processes such as ATP and pyrimidine biosynthesis.Atovaquone is approved for marketing in the US under the tradename Mepron® as tablets of 250 mg and an oral suspension which is indicated for the treatment and prophylaxis of infection. It is also available in combination with proguanil hydrochloride under the tradename Malarone® for the treatment and prevention of malaria.European Patent No. 123238 discloses 2-substituted-3-hydroxy-1,4-naphthoquinones, including atovaquone, which are said to be active against the human malaria parasite and also against species such as and , which are ...

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05-12-2013 дата публикации

Process for Industrial Production of 2-Methyl-1,4-Naphthaquinone

Номер: US20130324747A1
Принадлежит: TUBITAK

The present invention describes a process for producing 2-methyl-1,4-naphthoquinone by oxidizing 2-methylnaphthalene with fresh hydrogen peroxide in the presence of glacial acetic acid without any mineral or transition metal catalyst. 1. A process for producing 2-methyl-1 ,4-naphthoquinone by oxidation of 2-methylnaphthalene , including the steps of:a) oxidizing 2-methylnaphthalene with fresh 30% aqueous solution of hydrogen peroxide, wherein the molar ratio of 2-methylnaphthalene to hydrogen peroxide is in the range of 1:15 to 1:30 andb) oxidizing 2-methylnaphthalene in the presence of 17.4 N of glacial acetic acid, wherein the molar ratio of 2-methylnaphthalene to glacial acetic acid is in the range of 1:20 to 1:30.2. A process for producing 2-methyl-1 claim 1 ,4-naphthoquinone according to claim 1 , characterized in that the reaction time is in the period of 4-6 hours.3. A process for producing 2-methyl-1 claim 1 ,4-naphthoquinone according to claim 1 , characterized in that the reaction temperature is in the range of 70-90° C.4. A process for producing 2-methyl-1 claim 1 ,4-naphthoquinone according to claim 1 , characterized in that the oxidation reaction is carried out without any mineral acid or transition metal catalyst. The present invention relates to chemistry, pharmacy and vitamins.The industrial production of 2-methyl-1,4-naphthoquinone (menadione, vitamine K3) is a challenging problem because of its pharmacological activities. It is used as blood coagulating agent and as animal feed supplement. A lot of methods have been developed to oxidize 2-methylnaphthalene for the synthesis of 2-methyl-1,4-naphthoquinone.In a conventional process, 2-methylnapthalene is oxidized with stoichiometric amount of chromium (VI) compounds in sulfuric acid (Sheldon, Top. Curr. Chem., 164, 1993, 21). However, production of chromium salts are side products (18 kg of salt per kg of 2-methyl-1,4-naphthoquinone) and necessary treatment of this waste made it difficult to produce ...

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13-03-2014 дата публикации

PROCESS FOR THE PREPARATION OF A STABLE POLYMORPHIC FORM OF ATOVAGUONE

Номер: US20140073816A1
Принадлежит: TARO PHARMACEUTICAL INDUSTRIES LIMITED

The present invention provides a process for the preparation of a stable polymorph III of Atovaquone exhibiting characteristic peaks (expressed in degrees 2θ±0.2°θ) at about 6.9, 9.6, 14.1, 14.7, 17.0, 18.5, 19.1, 19.9, 20.3, 22.0, 22.6, 23.2, 24.2, 26.8, and 28.5, which comprises: (a) providing a sample of Atovaquone particles; (b) heating the sample of Atovaquone particles at a minimal temperature of between 140° C. to 160° C. depending on the particle size of the sample; and (c) cooling the sample to obtain the stable polymorphic form of Atovaquone. 1. A process for the preparation of a stable polymorph III of Atovaquone which comprises:(a) providing a sample of Atovaquone particles;(b) heating the sample of Atovaquone particles of step (a) at a temperature of at least about 160′C for a time sufficient of at least about one hour to obtain a stable polymorphic faun of Atovaquone, having characteristic peaks (expressed in degrees 20±0.2°θ) at approximately one or more of the positions: about 6.9, 9.6, 14.1, 14.7, 17.0, 18.5, 19.1, 19.9, 20.3, 22.0, 22.6, 23.2, 24.2, 26.8, and 28.5; and(c) cooling the sample of step (b).2. A process for the preparation of a stable polymorph III of Atovaquone which comprises:(a) providing a sample of Atovaquone particles wherein at least about 90% of the Atovaquone particles have a volume diameter of equal or less than about 40μ;(b) heating the sample of Atovaquone particles of step (a) at a temperature of at least about 140′C for a time sufficient to obtain a stable polymorphic form of Atovaquone, having characteristic peaks (expressed in degrees 20±0.2°θ) at approximately one or more of the positions: about 6.9, 9.6, 14.1, 14.7, 17.0, 18.5, 19.1, 19.9, 20.3, 22.0, 22.6, 23.2, 24.2, 26.8, and 28.5; and(c) cooling the sample of step (b).3. The process of claim 1 , wherein the Atovaquone particles of step (c) are further micronized if non-micronized particles are used in step (a) claim 1 , to obtain Atovaquone particles having ...

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07-01-2016 дата публикации

METHODS FOR SELECTIVE OXIDATION OF ALPHA TOCOTRIENOL IN THE PRESENCE OF NON-ALPHA TOCOTRIENOLS

Номер: US20160002138A1
Автор: MOLLARD Paul
Принадлежит:

A method of producing alpha-tocotrienol quinone or a stereoisomer thereof, the method comprising selective opening of alpha-tocotrienol chroman to alpha-tocotrienol quinone in the presence of non-alpha tocotrienol chromans by oxidizing alpha-to-cotrienol with a metal salt oxidizing agent, wherein the stoichiometric ratio of metal salt oxidizing agent/alpha-tocotrienol is at least 4:1 and wherein said metal oxidizing agent is added in sequential additions, in order to reduce oxidation of any amounts of non-alpha tocotrienol chromans that might have been present in the starting alpha-tocotrienol chroman material. This process uses conditions favoring oxidation rates of the alpha tocotrienol chroman vs. the non-alpha tocotrienol chromans. 2. The method according to comprising oxidizing alpha-tocotrienol with a metal salt oxidizing agent claim 1 , in a biphasic solution claim 1 , wherein the alpha-tocotrienol is dissolved in a non-polar solvent; the metal salt oxidizing agent is dissolved in a polar solvent; and the separate solutions are mixed to permit the oxidation.3. The method according to or claim 1 , wherein the metal salt oxidizing agent is an iron(III) salt selected from an iron(III) halide claim 1 , an iron(III) acetate claim 1 , an iron(III) citrate claim 1 , an iron(III) nitrate claim 1 , iron(III) tartrate or an iron(III) phosphate.4. The method according to or claim 1 , wherein the metal salt oxidizing agent is iron chloride (Fe(III)Cl).5. The method according to claim 4 , wherein the metal oxidizing agent is sufficient to oxidize at least about 98% of the alpha-tocotrienol chroman into the alpha-tocotrienol quinone.6. The method according to claim 5 , wherein the composition resulting from the oxidation has less than about 1% of one or more non-alpha-tocotrienol quinone compounds selected from alpha-tocotrienol claim 5 , beta-tocotrienol claim 5 , beta-tocotrienol quinone claim 5 , gamma-tocotrienol claim 5 , gamma-tocotrienol quinone claim 5 , delta- ...

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03-01-2019 дата публикации

Process for the production of alpha-tocotrienol and derivatives

Номер: US20190002428A1
Принадлежит: Bioelectron Technology Corp

The invention discloses novel processes for production, enrichment and/or isolation of alpha-tocotrienol from source material comprising at least one non-alpha-tocotrienol, such as natural extracts comprising mixed tocotrienols.

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21-01-2016 дата публикации

Process For The Preparation Of Substituted TRIS(2-Hydroxyphenyl)Methane

Номер: US20160016871A1
Принадлежит: Wintershall Holding GmbH

Described is a novel process for the preparation of substituted tris(2-hydroxyphenyl)methane derivatives and the use of tris(2-hydroxyphenyl)methane derivatives for tertiary mineral oil production.

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15-01-2015 дата публикации

METHOD FOR PREPARING A HERBICIDAL COMPOUND

Номер: US20150018569A1
Принадлежит: BANOR UNIVERSIITY

The present invention discloses a simple method for transforming cashew nut shell liquid into an active herbicidal composition. 2. The method of wherein R is alkyl having from 12 to 18 carbon atoms.3. The method of wherein R′ is alkyl having from 1 to 5 carbon atoms.4. The method of wherein R″ is hydrogen or alkyl having from 1 to 5 carbon atoms.6. The method of wherein alkylation step b) is carried out with alcohol R′OH wherein R′ is alkyl having up to 6 carbon atoms claim 1 , preferably methyl claim 1 , or with alkyl halide R′X wherein X is halogen claim 1 , or with alkyl sulfonate or alkyl sulfate claim 1 , or dialkyl sulfate claim 1 , optionally in a solvent.7. The method of wherein the alkylation step b) is carried out with dialkyl carbonate claim 6 , preferably dimethyl carbonate claim 6 , in the presence of a phase transfer catalyst.8. The method of wherein first oxidation step c) is carried out with oxygen claim 1 , or hydrogen peroxide claim 1 , or CrO claim 1 , or potassium permanganate claim 1 , or ferric chloride claim 1 , or potassium dichromate claim 1 , or nitric acid claim 1 , or with air in the presence of a catalyst selected from salcomine claim 1 , Pt claim 1 , Pd claim 1 , Ru claim 1 , Zr or Rh.9. The method of wherein Thiele (Thiele-Winter) acetoxylation step d) is carried out with acetic anhydride in the presence of sulfuric acid claim 1 , or triflic acid claim 1 , or bismuth triflate claim 1 , or acetic phosphoric anhydride or boron trifluoride.10. The method of wherein deacetylation step e) is carried out with lithium aluminium hydride or in the presence of a Lewis acid or with hydrochloric or another strong acid like sulphuric or para-toluenesulfonic acids in polar solvent.11. The method of wherein steps c claim 1 , d) claim 1 , and e) are replaced by a treatment with air or oxygen in the presence of a catalyst.12. The method of wherein the oxidizing is carried out with ferric chloride.13. The method of wherein the oxidizing is carried out ...

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17-01-2019 дата публикации

DEUTERATED IDEBENONE

Номер: US20190016657A1
Автор: Tung Roger D.
Принадлежит:

The present invention in one embodiment provides a compound of Formula I: 2. The compound of claim 1 , wherein each of R claim 1 , Rand Ris independently selected from CHand CD.3. The compound of claim 1 , wherein each Yis deuterium.4. The compound of claim 1 , wherein each Yis hydrogen.5. The compound of claim 1 , wherein each Yis hydrogen.6. The compound of claim 1 , wherein each Yis deuterium.7. The compound of claim 1 , wherein each Yis hydrogen.8. The compound of claim 1 , wherein each Yis deuterium.9. The compound of claim 1 , wherein Ris CH.10. The compound of claim 1 , wherein Ris CD.11. The compound of claim 1 , wherein Ris CH.12. The compound of claim 1 , wherein Ris CD.13. The compound of claim 1 , wherein Ris CH.14. The compound of claim 1 , wherein Ris CD.15. The compound of claim 1 , wherein each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; and each Yis deuterium.19. The compound of claim 1 , wherein any atom not designated as deuterium is present at its natural isotopic abundance.20. A pharmaceutical composition comprising the compound of or a pharmaceutically acceptable salt thereof; and a pharmaceutically acceptable carrier.21. A method of reducing oxidative toxicity in mitochondria claim 1 , comprising contacting mitochondria with a compound of .22. A method of treating a condition that is Duchenne's muscular dystrophy or multiple sclerosis claim 1 , comprising administering to a subject in need of such treatment a compound of .23. The method of claim 22 , wherein the condition is primary progressive multiple sclerosis. This application is a continuation of U.S. application Ser. No. 14/414,039, filed on Jan. 9, 2015, which is the U.S. National Stage of International Application No. PCT/US2013/050302, filed on Jul. 12, 2013, published in English, which claims the benefit of U.S. Provisional Application No. 61/670,716, ...

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28-01-2021 дата публикации

Aminated lignin-derived compounds and uses thereof

Номер: US20210024453A1
Принадлежит: Cmblu Energy Ag, CMBLU PROJEKT AG

The present invention relates to novel lignin-derived compounds and compositions comprising the same and their use as redox flow battery electrolytes. The invention further provides a method for preparing said compounds and compositions as well as a redox flow battery comprising said compounds and compositions. Additionally, an assembly for carrying out the inventive method is provided.

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09-02-2017 дата публикации

PROCESS FOR THE PRODUCTION OF ALPHA-TOCOTRIENOL AND DERIVATIVES

Номер: US20170037023A1
Принадлежит:

The invention discloses novel processes for production, enrichment and/or isolation of alpha-tocotrienol from source material comprising at least one non-alpha-tocotrienol, such as natural extracts comprising mixed tocotrienols. 1. A process for the production , enrichment and/or isolation of alpha-tocotrienol from a plant extract that comprises at least one non-alpha tocotrienol and that optionally comprises alpha-tocotrienol , optionally comprises alpha-tocopherol and optionally comprises other tocols , non-tocols and/or organic impurities , comprising the steps of:1a.) reacting the plant extract with suitable reagents which react with the one or more non-alpha-tocols to introduce a functional group in the free 5 and/or 7 position of the one or more non-alpha-tocols;1b.) separating the one or more non-alpha-tocols that have been functionalized in step (1a) from the optional alpha-tocotrienol and optional alpha tocopherol and optional non-tocol compounds that may be present;1c.) optionally further separating the alpha-tocotrienol in the mixture separated in step (1b), from the optional alpha tocopherol and from optional non-tocols;1d.) chemically reacting the separated one or more non-alpha-tocols that have been functionalized from step (1b) to give alpha-tocotrienol; and1e.) optionally combining the alpha-tocotrienol from step (1c) with the alpha-tocotrienol from step (1d) to give alpha-tocotrienol,wherein step 1a.) comprises amino-alkylation performed with a formaldehyde equivalent and 1-methylpiperazine, followed by acidification;and wherein step 1d.) comprises reduction performed with sodium cyano borohydride.2. The process of claim 1 , wherein the plant extract is selected from the group consisting of a palm oil extract claim 1 , a palm fruit extract claim 1 , a rice extract claim 1 , a rice bran extract claim 1 , a barley extract claim 1 , an annatto extract claim 1 , and a mixture thereof.3. The process of claim 2 , wherein the plant extract is a palm oil ...

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24-02-2022 дата публикации

REDOX-ACTIVE THERAPEUTICS FOR TREATMENT OF MITOCHONDRIAL DISEASES AND OTHER CONDITIONS AND MODULATION OF ENERGY BIOMARKERS

Номер: US20220055975A1
Принадлежит:

Methods of treating or suppressing mitochondrial diseases, such as Friedreich's ataxia (FRDA), Leber's Hereditary Optic Neuropathy (LHON), mitochondrial myopathy, encephalopathy, lactacidosis, stroke (MELAS), or Kearns-Sayre Syndrome (KSS) are disclosed, as well as compounds useful in the methods of the invention, such as alpha-tocopherol quinone. Methods and compounds useful in treating other disorders are also disclosed. Energy biomarkers useful in assessing the metabolic state of a subject and the efficacy of treatment are also disclosed. Methods of modulating, normalizing, or enhancing energy biomarkers, as well as compounds useful for such methods, are also disclosed. 2. (canceled)3. (canceled)4. (canceled)6. A method of treating a mitochondrial disorder claim 5 , modulating one or more energy biomarkers claim 5 , normalizing one or more energy biomarkers claim 5 , or enhancing one or more energy biomarkers claim 5 , comprising administering to a subject a therapeutically effective amount or effective amount of one or more compounds of .13. A method of treating a mitochondrial disorder claim 12 , modulating one or more energy biomarkers claim 12 , normalizing one or more energy biomarkers claim 12 , or enhancing one or more energy biomarkers claim 12 , by administering to a subject a therapeutically effective amount or effective amount of one or more compounds of .16. A method of treating a mitochondrial disorder claim 15 , modulating one or more energy biomarkers claim 15 , normalizing one or more energy biomarkers claim 15 , or enhancing one or more energy biomarkers claim 15 , by administering to a subject a therapeutically effective amount or effective amount of one or more compounds of .18. (canceled)19. The method of claim 6 , wherein the mitochondrial disorder is selected from the group consisting of inherited mitochondrial diseases; Myoclonic Epilepsy with Ragged Red Fibers (MERRF); Mitochondrial Myopathy claim 6 , Encephalopathy claim 6 , Lactacidosis ...

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02-03-2017 дата публикации

EFFICIENT SCALABLE SYNTHESES OF ABSCISIC ACID, 8'-ACETYLENE ABSCISIC ACID AND 8'-CYCLOPROPYL ABSCISIC ACID

Номер: US20170057899A1
Принадлежит: NATIONAL RESEARCH COUNCIL OF CANADA

Methods are provided for synthesis of abscisic acid and 8′ analogues thereof (including an enantiopure 8′-acetylene analogue) including methods wherein the previously reported first step of oxidation of 2,6-dimethylphenol (VI) to 2,6-dimethylbenzoquinone, mono ketal (VII) is replaced by a novel two step process comprising (i) oxidation of 2,6-dimethylphenol (VI) using potassium peroxymonosulfate with a catalytic amount of iodobenzene to produce 2,6-dimethylbenzoquinone (XVI) and (ii) ketalization of 2,6-dimethylbenzoquinone (XVI) using ethylene glycol, trimethylorthoformate with a catalytic amount of p-toluenesulfonic acid to produce 2,6-dimethylbenzoquinone, mono ketal (VII). 2. The method of wherein the reduction at step c is performed using Red Al.3. The method of wherein the organic acid is acetic acid and the alcohol is methanol.4. The method of wherein R is a methyl group and the carbanion magnesium halide is methylmagnesium chloride.5. The method of wherein R is a cycloproply group and the carbanion magnesium halide is cyclopropylmagnesium bromide.6. The method of wherein R is an alkynyl group and the carbanion magnesium halide is ethynylmagnesium chloride.8. The method of wherein the reduction at step c is performed using Red Al.9. The method of wherein the organic acid is acetic acid and the alcohol is methanol.10. The method of wherein R is an alkynyl group and the carbanion magnesium halide is ethynylmagnesium chloride.11. The method of wherein the organic or inorganic salt is lithium triflate. This application claims the benefit of U.S. Provisional Application No. 62/210,477 filed Aug. 27, 2015.The invention relates, in general, to the field of plant hormones and, in particular, to a method of synthesizing abscisic acid, 8′-acetylene abscisic acid and 8′-cyclopropyl abscisic acid.Abscisic acid (ABA, I) is a plant hormone that regulates diverse aspects of growth and development. In higher plants including seed germination and maturation, regulation of ...

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29-05-2014 дата публикации

TICKET PRODUCTION DEVICE AND TICKET PRODUCTION METHOD

Номер: US20140148335A1
Принадлежит: SEIKO EPSON CORPORATION

A ticket production device that cuts continuous recording paper printed with information and produces a ticket includes a paper conveyance means that conveys the recording paper through a paper conveyance path; a printing means that prints information on the recording paper conveyed by the paper conveyance means; a paper cutting means that cuts the recording paper on which information was printed into a ticket of a specific length; a paper position detection means that detects the position of the recording paper waiting at a paper exit; and a control means that integrally controls these other means. When the paper position detection means detects the position of the recording paper changed, the control means operates the paper cutting means and produces a ticket based on the detection result from the paper position detection means. 1. A ticket production device configured to cut and issue a continuous recording paper on which information is printed as a ticket from a paper exit , comprising:a paper conveyance means configured to convey the recording paper through a paper conveyance path;a print means configured to print information on the recording paper conveyed by the paper conveyance means;a paper cutting means configured to cut the recording paper printed with information into a ticket of a specific length;a paper position detection means configured to detect change in the position of the recording paper waiting at the paper exit; anda control means configured to integrally control each of the other means;the paper position detection means is configured to detect whether the position of the recording paper changed, andthe control means is configured to operate the paper cutting means to produce the ticket based on the detection result of the paper position detection means.2. The ticket production device described in claim 1 , wherein:the paper position detection means is configured to detect change in the position of the recording paper at least in a direction ...

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12-06-2014 дата публикации

Image recording system and image recording method

Номер: US20140158771A1
Принадлежит: Ricoh Co Ltd

Provided is an image recording system for recording an image on a thermally reversible recording medium held by a conveyed article conveyed on a predetermined conveying path in a predetermined conveying direction, including: a recording device provided on at least one side of the conveying path in a direction perpendicular to the conveying direction and configured to record an image on the thermally reversible recording medium of the conveyed article conveyed to a position facing the recording device by heating the thermally reversible recording medium. The image includes a scan image to be read by a reading device when the conveyed article is conveyed downstream in the conveying direction from the position facing the recording device. The recording device records the scan image on the thermally reversible recording medium within a former half of a recording time of the image.

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26-03-2015 дата публикации

TREATMENT FOR BREAST TUMOR CELL METASTASIS

Номер: US20150087722A1
Принадлежит:

A method for inhibiting or preventing metastasis of breast tumor cells in a subject is disclosed. The method includes administering to the subject an effective amount of a compound of formula (I). In formula (I), R is H or methyl. 2. The method for inhibiting or preventing metastasis of breast tumor cells in the subject of claim 1 , wherein the breast tumor cells are tested negative for estrogen receptors (ER−) claim 1 , progesterone receptors (PR−) claim 1 , and human epidermal growth factor receptors 2 (HER2−).3. The method for inhibiting or preventing metastasis of breast tumor cells in the subject of claim 1 , wherein the breast tumor cells are tested positive for estrogen receptors (ER+). This application is a continuation-in-part (CIP) of U.S. patent application Ser. No. 13/430,703 filed on Mar. 27, 2012 which claims priority to Taiwan Application Serial Number 101105469, filed on Feb. 20, 2012. The entire disclosures of both applications are hereby incorporated by reference herein.1. Technical FieldThe present disclosure relates to a method for inhibiting or preventing metastasis. More particularly, the present disclosure relates to a method for inhibiting or preventing breast tumor cell metastasis.2. Description of Related ArtAccording to statistics, every year 250 thousand people died from the breast tumor over world. In Taiwan for female tumor the incidence rate of breast tumor is the second highest. From 1990 to 1991 in Taiwan the number of people died from tumor is increased to 32,993, which is increased by 3.83% in one year and occupies 26.05% of the death rate. The breast tumor is one of the ten lethal tumors, and the incidence rate of breast tumor tends to increase gradually. The age of onset in Taiwan is younger than that in occident countries. Every year about 1,200 women are died from the breast tumor. Thus the breast tumor greatly threatens the health of women. The incident of cancer is closely associated with the gene and the acquired environment ...

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19-06-2014 дата публикации

MULTI-FUNCTION SYSTEM FOR RECOVERING MEDIA PRINTED WITH THERMO-REACTIVE INK

Номер: US20140171307A1
Принадлежит: XEROX CORPORATION

What is disclosed is a multi-function system which receives media printed with ink having thermo-reactive properties with the ink being visually transparent on that media, and which processes that media such that the ink becomes visually perceptible. One embodiment of the present system comprises an input tray for receiving printed media into a transport path along which the media travels. A cooling element resides in proximity to that transport path for changing a temperature T of the media to T≦T. A temp-normalizing element is positioned along the transport path downstream of the cooling element for changing a temperature of the media such that the media's temperature T can be normalized back to a temperature range T Подробнее

19-04-2018 дата публикации

Concerted processes for forming 1,2,4-trihydroxybenzene from hydroquinone

Номер: US20180105544A1
Принадлежит: Lockheed Martin Energy LLC

Flow batteries incorporating an active material with one or more catecholate ligands can have a number of desirable operating features. Commercial syntheses of catechol produce significant quantities of hydroquinone as a byproduct, which presently has limited value in the battery industry and can represent a significant waste disposal issue at industrial production scales. Using a concerted, high-yield process, low-value hydroquinone can be transformed into high-value 1,2,4-trihydroxybenzene, which can be a desirable ligand for active materials of relevance in the flow battery industry. Methods for forming 1,2,4-trihydroxybenzene can include: oxidizing hydroquinone in a first reaction to form p-benzoquinone, converting the p-benzoquinone in a second reaction to form 1,2,4-triacetoxybenzene, deacetylating the 1,2,4-triacetoxybenzene in a third reaction to form 1,2,4-trihydroxybenzene, and isolating the 1,2,4-trihydroxybenzene after performing the first reaction, the second reaction and the third reaction consecutively.

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30-04-2015 дата публикации

Process for the preparation of pillar[5]quinone

Номер: US20150119605A1

The present invention relates to a process for the preparation of pillar[5]quinone and further relates to an easy-to-operate and chromatography-free process for the preparation of crystalline pillar [5] quinone by the oxone/iodobenzene-mediated oxidative de-aromatization of readily available 1,4-dimethoxypillar[5] arenes in good

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27-04-2017 дата публикации

PROCESS FOR PRODUCING HYDROQUINONE AND DERIVATES

Номер: US20170113991A1
Принадлежит:

The present disclosure relates to an improved, environmentally friendly, process for producing compounds such as hydroquinone (benzene-1,4-diol) and its derivatives. The process can be carried out at ambient temperature and pressure using a recyclable copper catalyst and recyclable intermediate materials. The process generally entails reacting an aromatic compound such as benzene with hydrogen peroxide in the present of a pure elemental copper catalyst or a copper (I) salt catalyst to form oxidation product such as benzoquinone, and reducing the compound to hydroquinone or a hydroquinone derivative. 19-. (canceled)10. A process for producing hydroquinone comprising reacting benzene with hydrogen peroxide in the presence of elemental copper catalyst or a copper(I) salt catalyst to form oxidation product comprising benzoquinone and phenol , and converting the oxidation product to hydroquinone by reduction , provided that the selectivity for hydroquinone from benzene is greater than 60%.11. The process according to claim 10 , wherein the catalyst is a copper(I) salt catalyst and the copper (I) salt catalyst is a tetrakis(acetonitrile)copper(I) salt having the following formula:{'br': None, 'sub': 3', '4, 'Cu(CHCN)-A,'}wherein A is an anion.12. The process of claim 11 , wherein the anion is selected from the group consisting of ClO claim 11 , NO claim 11 , BF claim 11 , PF claim 11 , and CFSO.13. (canceled)14. The process of carried out at a temperature of from 10° C. to 80° C.15. The process of claim 10 , wherein the reaction of benzene with hydrogen peroxide is carried out in a solvent.16. The process of claim 15 , wherein the solvent is selected from the group consisting of nitrile claim 15 , a C-Cketone claim 15 , a C-Cether claim 15 , a C-Cester claim 15 , and a C-Chydrocarbon.17. The process of claim 16 , wherein the nitrile is selected from the group consisting of acetonitrile claim 16 , propionitrile claim 16 , butanenitrile claim 16 , and benzonitrile.18. A ...

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07-05-2015 дата публикации

METHOD OF PREPARATION OF STEREOSPECIFIC QUINONE DERIVATIVES

Номер: US20150126763A1
Принадлежит:

The description provides processes for the regio and stereospecific synthesis of polyprenylatedquinone derivatives, such as Vitamin K1, K2 and Ubiquinone, exploiting dithioacetals, especially 1,3-dithiane, mediated Umpolung chemistry which works along a new concept “Inhibiting resonance delocalization (IRD)” to overcome isomerization generated due to delocalization of allyliccarbanion on the π-electron cloud of an allylic systems by the conventional synthesis. 2. The method of wherein the said quinone derivatives are selected from the group consisting of coenzyme Q10 claim 1 , vitamin K1 claim 1 , vitamins K2-4 claim 1 , K2-6 claim 1 , K2-7 claim 1 , K2-8 and K2-9. Under 35 U.S.C. §119(e) this application claims the benefit of U.S. Provisional Application No. 61/962,169, filed Nov. 1, 2013 titled: Method of Preparation of Stereospecific Quinone Derivatives, which is hereby incorporated by reference in their entirety for all purposes.The present disclosure relates to regio- and stereospecific synthesis of quinone derivatives, attached with polyprenyl side chain, to yield various natural equivalent vitamins, e.g., vitamin K and ubiquinone.Current knowledge of stereochemistry demands responsible drug development. Most proteins, nucleic acids, polysaccharides, lipids and steroids are chiral. In other words, almost all of the main therapeutic targets are chiral and, therefore, show stereospecific interactions with endogenous and exogenous ligands. Stereo selectivity of interaction is a well-recognized criterion of specific drug-receptor interactions. Such stereoselectivity has been observed with all classes of receptors, with both physiological and non-physiological ligands. However, pharmacological implications of this have not always been appreciated, especially the toxicity aspects.It is not always possible to determine the long term toxic effects of the minor quantities of unintended isomers in a product by conventional acute and chronic toxicity studies. This minor ...

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14-05-2015 дата публикации

DEACTIVATION OF URUSHIOL AND METHOD OF TREAMENT AND PREVENTION OF CONTACT DERMATITIS

Номер: US20150132811A1
Автор: Braslau Rebecca
Принадлежит:

The invention herein disclosed provides for compositions, methods for synthesizing said compositions, and methods for using said compositions, wherein the compositions and methods may be used to bind to and/or deactivate a poison oak oil, such as urushiol. The compositions and methods can be used to treat and/or reduce an inflammatory reaction and/or hypersensitivity to natural compounds found in poison oak, poison ivy, poison sumac, mango, lac tree, cashew nut, and Asian lacquer. 125-. (canceled)26. A method for deactivating a catechol in a sample , the method comprising the steps of (i) contacting an oxidant with the sample (ii) allowing the oxidant to react with the catechol in the sample thereby creating an orthoquinone; (iii) allowing the orthoquinone to react with the oxidant thereby generating a polymer; the method resulting in deactivating the catechol in the sample.27. The method of claim 26 , further comprising a catalyst.28. The method of claim 27 , wherein the catalyst is a metal.29. The method of claim 27 , wherein the catalyst is a nitroxide.30. The method of claim 27 , wherein the catalyst is a nitroxide precursor.31. The method of claim 27 , wherein the catalyst is an enzyme.32. The method of claim 27 , wherein the oxidant is a natural atmospheric gas.33. The method of claim 28 , wherein the metal catalyst is selected from the group consisting of iron claim 28 , copper claim 28 , cobalt claim 28 , nickel claim 28 , palladium claim 28 , rhodium claim 28 , ruthenium claim 28 , manganese claim 28 , and platinum.34. The method of claim 29 , wherein the nitroxide is selected from the group consisting of alkyl nitroxide claim 29 , Fremy's salt claim 29 , and acyl nitroxide.35. The method of wherein the nitroxide is tetramethylpiperidinyloxy (TEMPO).36. The method of claim 30 , wherein the nitroxide precursor is selected from the group consisting of an amine and a hydroxamic acid.37. The method of claim 31 , wherein the enzyme is selected from the group ...

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07-08-2014 дата публикации

PROCESS FOR THE PRODUCTION OF ALPHA-TOCOTRIENOL AND DERIVATIVES

Номер: US20140221674A1
Принадлежит: Edison Pharmaceuticals, Inc.

The invention discloses novel processes for production, enrichment and/or isolation of alpha-tocotrienol from source material comprising at least one non-alpha-tocotrienol, such as natural extracts comprising mixed tocotrienols. 1. A process for the production , enrichment and/or isolation of d-alpha-tocotrienol from a plant extract that comprises at least one non-alpha tocotrienol and that optionally comprises alpha-tocopherol and optionally comprises other tocols , non-tocols and/or organic impurities , comprising the steps of:1a.) reacting the plant extract with suitable reagents which react with the one or more non-alpha-tocols to introduce a functional group in the free 5 and/or 7 position of the one or more non-alpha-tocols;1b.) separating the one or more non-alpha-tocols that have been functionalized in step (1a) from the alpha-tocotrienol and optional alpha tocopherol and other non-tocol compounds that may be present;1c.) optionally further separating the alpha-tocotrienol in the mixture separated in step (1b), from the optional alpha tocopherol and from optional other non-tocols;1d.) chemically reacting the separated one or more non-alpha-tocols that have been functionalized from step (1b) to give alpha-tocotrienol; and1e.) optionally combining the alpha-tocotrienol from step (1c) with the alpha-tocotrienol from step (1d) to give alpha-tocotrienol.2. The process of claim 1 , wherein the plant extract is selected from a palm oil extract claim 1 , a palm fruit extract claim 1 , a rice extract claim 1 , a rice bran extract claim 1 , a barley extract claim 1 , an annatto extract claim 1 , or a mixture thereof.3. The process of claim 2 , wherein the plant extract is a palm oil extract.4. The process of claim 2 , wherein the plant extract is Tocomin®.5. The process of claim 1 , where the reaction in step (1a) is amino-alkylation followed by acidification.6. The process of claim 5 , where the amino-alkylation is performed with paraformaldehyde and a cyclic amine ...

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04-06-2015 дата публикации

Electronic Handwriting Processing Device And Method Thereof

Номер: US20150151558A1
Автор: Hwang Jih-Shang
Принадлежит:

An electronic handwriting processing method, used to process handwriting written on a writing medium with temperature-dependent color ink, including following steps: provide a temperature varying element; apply said temperature varying element, so that it reaches temperature to make said temperature-dependent color ink to change from a first color to a second color; and contact said handwriting with said temperature varying element, to change its color from said first color to said second color, wherein, one of said first color and said second color is visible, while the other is transparent. An electronic handwriting processing device is also disclosed. 1. An electronic handwriting processing method , used to process handwriting written on a writing medium with temperature-dependent color ink , including following steps:provide a temperature varying element;apply said temperature varying element, so that it reaches temperature to make said temperature-dependent color ink to change from a first color to a second color; andcontact said handwriting with said temperature varying element, to change color of said handwriting from said first color to said second color, wherein, one of said first color and said second color is visible, while the other is transparent.2. The electronic handwriting processing method as claimed in claim 1 , comprising further following steps:apply said temperature varying element, so that it reaches temperature to make said temperature-dependent color ink to change from said second color to said first color; andcontact said handwriting with said temperature varying element, to change its color from said second color to said first color.3. An electronic handwriting processing device claim 1 , used in said electronic handwriting processing method as claimed in claim 1 , said electronic handwriting processing device comprising:a power supply; anda temperature varying element, connected electrically to said power supply, to use power provided by ...

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25-05-2017 дата публикации

IMAGE FORMING APPARATUS

Номер: US20170146921A1
Автор: SUZUKI Tomomi
Принадлежит:

An image forming apparatus comprises a sensor configured to detect on a sheet an image with a decolorable recording agent containing a coloring material to be decolored from the sheet; a printer configured to carry out a printing operation of an image formed with the decolorable recording agent and a printing operation of an image formed with a non-decolorable recording agent containing a coloring material that is not decolored; and a controller configured to control the printer to execute the printing operation with the decolorable recording agent on the sheet in a case in which the image is detected by the sensor. 1. An image forming apparatus , comprising:a sensor configured to detect on a sheet an image with a decolorable recording agent comprising a coloring material;a printer configured to carry out a printing operation of an image formed with the decolorable recording agent and a printing operation of an image formed with a non-decolorable recording agent comprising a coloring material; anda controller configured to control the printer to execute the printing operation with the decolorable recording agent on the sheet in a case in which the image formed with the non-decolorable recording agent or decolorable recording agent is detected by the sensor.2. The image forming apparatus according to claim 1 , whereinthe printer prints the image in a predetermined area of the sheet in a case in which the printing with the decolorable recording agent is carried out.3. The image forming apparatus according to claim 1 , whereinthe controller controls the printer to carry out the printing with the non-decolorable recording agent on the sheet in a case in which the image is detected by the sensor.4. The image forming apparatus according to claim 2 , whereinthe controller controls the printer to carry out the printing with the non-decolorable recording agent on the sheet in a case in which the image is detected by the sensor.5. The image forming apparatus according to ...

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22-09-2022 дата публикации

NEW TELESCOPING SYNTHESES OF 2-METHOXYMETHYL-P-PHENYLENEDIAMINE

Номер: US20220298101A1
Принадлежит:

The invention relates to processes for preparing 2-methoxymethyl-p-phenylenediamine (I), cosmetically acceptable salts thereof, or mixtures thereof. 1. A process for preparing 2-methoxymethyl-p-phenylenediamine (I) , a cosmetically acceptable salt thereof , or mixture thereof , the process comprising the steps of:(a) providing 2-methoxymethyl-1,4-benzochinone (IV);(b) condensing 2-methoxymethyl-1,4-benzochinone (IV) with an amine source NH2R1 to form 2-(methoxymethyl)-N1(R1),N4(R1)-cyclohexa-2,5-diene-1,4-diimine (Va); and(c) reacting 2-(methoxymethyl)-N1(R1),N4(R1)-cyclohexa-2,5-diene-1,4-diimine (Va) in the presence of a hydrogen source to form 2-methoxymethyl-p-phenylenediamine (I).2. The process of claim 1 , wherein moiety R1 of amine source NH2-R1 is selected from OH claim 1 , NH2 claim 1 , linear or branched (C1-C6)alkyl which optionally may be substituted with OH claim 1 , linear or branched (C1-C6)alkylene-(C5-C6)cycloalkyl and linear or branched (C1-C6)alkylbenzol claim 1 ,3. The process of claim 1 , wherein step (b) comprises condensing 2-methoxymethyl-1 claim 1 ,4-benzochinone (IV) with hydroxylamine NHOH to form bis-oxime 2-(methoxymethyl)-cyclohexa-2 claim 1 ,5-diene-1 claim 1 ,4-dione oxime (Vb) claim 1 , and wherein step (c) comprises reacting (Vb) to form (I).4. The process of any of to claim 1 , wherein step (a) comprises:(a1) alkylating 1,4-benzoquinone (VIII) in the presence of 2-methoxyacetic acid (IX) to form a mixture of 2-methoxymethyl-1,4-benzochinone (IV) and 1,4-benzoquinone (VIII); and(a2) removing 1,4-benzoquinone (VIII).5. The process of claim 4 , wherein removing 1 claim 4 ,4-benzoquinone (VIII) in step (a2) is carried out by water vapour distillation or short path distillation or thin-film evaporation.6. The process of any of to claim 4 , wherein step (a) comprises:(a3) providing 2-methyl-1,4-benzochinone (II);(a4) brominating 2-methyl-1,4-benzochinone (II) to form 2-bromomethyl-1,4-benzochinone (III); and(a5) etherifying 2-bromomethyl ...

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18-06-2015 дата публикации

Deuterated Idebenone

Номер: US20150166449A1
Автор: Tung Roger D.
Принадлежит: CONCERT PHARMACEUTICALS, INC.

The present invention in one embodiment provides a compound of Formula I:(I), or a pharmaceutically acceptable salt thereof, wherein the variables shown in Formula I are as defined in the specification. 2. The compound of claim 1 , wherein each of R claim 1 , Rand Ris independently selected from CHand CD.3. The compound of claim 1 , wherein each Yis deuterium.4. The compound of claim 1 , wherein each Yis hydrogen.5. The compound of claim 1 , wherein each Yis hydrogen.6. The compound of claim 1 , wherein each Yis deuterium.7. The compound of claim 1 , wherein each Yis hydrogen.8. The compound of claim 1 , wherein each Yis deuterium.9. The compound of claim 1 , wherein Ris CH.10. The compound of claim 1 , wherein Ris CD.11. The compound of claim 1 , wherein Ris CH.12. The compound of claim 1 , wherein Ris CD.13. The compound of claim 1 , wherein Ris CH.14. The compound of claim 1 , wherein Ris CD.15. The compound of or claim 1 , wherein each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; and each Yis deuterium.19. The compound of claim 1 , wherein any atom not designated as deuterium is present at its natural isotopic abundance.20. A pharmaceutical composition comprising the compound of or a pharmaceutically acceptable salt thereof; and a pharmaceutically acceptable carrier.21. A method of reducing oxidative toxicity in mitochondria claim 1 , comprising contacting mitochondria with a compound of .22. A method of treating a condition that is Duchenne's muscular dystrophy or multiple sclerosis claim 1 , comprising administering to a subject in need of such treatment a compound of .23. The method of claim 22 , wherein the condition is primary progressive multiple sclerosis.24. A method of treating a condition that is Duchenne's muscular dystrophy or multiple sclerosis claim 20 , comprising administering to a subject in need of such treatment a ...

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04-09-2014 дата публикации

METHODS FOR SELECTIVE OXIDATION OF ALPHA TOCOTRIENOL IN THE PRESENCE OF NON-ALPHA TOCOTRIENOLS

Номер: US20140249332A1
Автор: MOLLARD Paul
Принадлежит:

A method of producing alpha-tocotrienol quinone or a stereoisomer thereof, the method comprising selective opening of alpha-tocotrienol chroman to alpha-tocotrienol quinone in the presence of non-alpha tocotrienol chromans by oxidizing alpha-tocotrienol with a metal salt oxidizing agent, wherein the stoichiometric ratio of metal salt oxidizing agent/alpha-tocotrienol is at least 4:1 and wherein said metal oxidizing agent is added in sequential additions, in order to reduce oxidation of any amounts of non-alpha tocotrienol chromans that might have been present in the starting alpha-tocotrienol chroman material. This process uses conditions favoring oxidation rates of the alpha tocotrienol chroman vs the non-alpha tocotrienol chromans. 2. The method according to comprising oxidizing alpha-tocotrienol with a metal salt oxidizing agent claim 1 , in a biphasic solution claim 1 , wherein the alpha-tocotrienol is dissolved in a non-polar solvent; the metal salt oxidizing agent is dissolved in a polar solvent; and the separate solutions are mixed to permit the oxidation.3. The method according to claim 1 , wherein the metal salt oxidizing agent is an iron(III) salt selected from an iron(III) halide claim 1 , an iron(III) acetate claim 1 , an iron(III) citrate claim 1 , an iron(III) nitrate claim 1 , iron(III) tartrate or an iron(III) phosphate.4. The method according to claim 1 , wherein the metal salt oxidizing agent is iron chloride (Fe(III)Cl).5. The method according to claim 4 , wherein the metal oxidizing agent is sufficient to oxidize at least about 98% of the alpha-tocotrienol chroman into the alpha-tocotrienol quinone.6. The method according to claim 5 , wherein the composition resulting from the oxidation has less than about 1% of one or more non-alpha-tocotrienol quinone compounds selected from alpha-tocotrienol claim 5 , beta-tocotrienol claim 5 , beta-tocotrienol quinone claim 5 , gamma tocotrienol claim 5 , gamma-tocotrienol quinone claim 5 , delta-tocotrienol ...

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23-07-2015 дата публикации

METHOD FOR PRODUCING CRESOL FROM PHENOL AND METHANOL VIA GAS PHASE ALKYLATION

Номер: US20150203425A1

The present invention relates to a method for producing cresol from phenol and methanol via gas phase alkylation, in which phenol and methanol are preheated and mixed with diluent gas, then the mixture continuously go through a catalyst bed comprising the catalyst for alkylation of phenol with methanol, to produce cresol by gas phase reaction at the reaction temperature of 200-500° C. and the weight hourly space velocity of 0.5˜20 h. The catalyst for alkylation of phenol with methanol is obtained by modification steps and using ZSM-5 zeolite, MCM-22 zeolite or Beta zeolite as an active composition. Using phenol and methanol as feedstock, the cresol selectivity can reach to 90%, and the p-cresol selectivity can reach to 58%. The catalyst is environmental friendly and non-corrosive to the equipment with a good stability and a broad prospect in industrial application. 1. A method for producing cresol from phenol and methanol via gas phase alkylation , in which phenol and methanol are preheated and mixed with a diluent gas , then continuously going through a catalyst bed comprising the catalyst for alkylation of phenol with methanol , to produce cresol by gas phase reaction at a reaction temperature from 200° C. to 500° C. and a weight hourly space velocity from 0.5 hto 20 h; wherein the preparation of said catalyst comprise a forming step by mixing a binder with an active component consisted of molecular sieve , and a modification step by using at least one of an acid , a silanization reagent or a steam treatment to adjust the acid sites.2. A method for producing cresol from phenol and methanol via gas phase alkylation according to claim 1 , wherein the preparation of said catalyst comprises an oxide modification step.3. A method for producing cresol from phenol and methanol via gas phase alkylation according to claim 1 , wherein the weight percentage of the molecular sieve in said catalyst is at a range from 60 wt % to 85 wt % claim 1 , and the weight percentage of ...

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13-07-2017 дата публикации

PREPARATION OF 2,6- AND 2,7-DISUBSTITUTED ANTHRAQUINONE DERIVATIVES

Номер: US20170197830A1
Принадлежит: BASF SE

The present invention relates to novel anthraquinone derivatives, 2,6-diisohexylanthracene-9,10-dione and 2,7-diisohexyl-anthracene-9,10-dione, preferably to be used for the preparation of hydrogen peroxide, and to a process for the preparation of these anthraquinone derivatives. 4. The composition of claim 3 , wherein at least 90 weight % of the composition consist of the compounds of formula (Ia) and formula (Ib).5. The composition of claim 3 , wherein a molar ratio of the compound of formula (Ia) relative to the compound of formula (Ib) is in a range of from 0.2:1 to 5:1.6. The composition of claim 3 , having a solubility of at least 1.0 mol/l in a solvent mixture of which at least 99.9 weight-% consist of ortho-xylene and diisobutyl carbinol with a molar ratio of the ortho-xylene relative to the diisobutyl carbinol in a range of from 0.99:1 to 1.01:1 claim 3 , wherein said solubility refers to a molar amount of the compound of formula (Ia) plus a molar amount of the compound of formula (Ib) dissolved in 1 l of the solvent mixture at a temperature of from 20 to 23° C. and at a pressure of from 0.9 to 1.1 bar.7. The composition of claim 3 , wherein at least 90 weight % of the compound of formula (Ia) and at least 96 weight % of the compound of formula (Ib) are present in solid form.8. The composition of claim 3 , being at least partially dissolved in a solvent.12. The process of claim 11 , wherein the reacting (b) is carried out in a solvent.13. The process of claim 11 , further comprising: after (b) and prior to (c) claim 11 ,(b′) separating the compounds of formula (Va) and/or formula (Vb) from the mixture obtained in (b), thereby obtaining a mixture comprising the compounds of formula (Va) and/or formula (Vb).14. The process of claim 11 , wherein prior to (c) claim 11 , the compounds of formula (Va) and/or formula (Vb) are not separated from the mixture obtained in (b).15. The process of claim 11 , wherein the oxidation reaction in (c) is carried out in a ...

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30-07-2015 дата публикации

PROCESS FOR THE PREPARATION OF VITAMIN K2

Номер: US20150210620A1
Принадлежит:

Using a combination of Kumada, Suzuki and Biellmann chemistry, various menaquinones can synthesised rapidly and with stereochemical integrity offering a new way of preparing these vitamin K2 components for the pharmaceutical market. In one embodiment a process for the preparation of a compound of formula (I) 19-. (canceled)13. The process as claimed in wherein conversion is achieved using cerium ammonium nitrate.15. The process as claimed in wherein the deprotonation step (i) is achieved using BuLi.16. The process as claimed in wherein Ar is Ph.17. The process as claimed in wherein LG is a halide.18. The process as claimed in wherein the step (iii) reduction uses cerium ammonium nitrate.19. The process as described in wherein the compound of formula (I) is MK-7. This application is a continuation of U.S. application Ser. No. 13/119,585, filed Apr. 19, 2011 (U.S. Pat. No. 9,012,693) which is the U.S. national phase of International Application No. PCT/GB2009/002282 filed 24 Sep. 2009, which designated the U.S. and claims priority to GB Application No. 0817528.3 filed 24 Sep. 2008, the entire contents of each of which are hereby incorporated by reference.This application relates to the synthesis of a compound that forms part of vitamin K2, as well as the synthesis of some novel intermediate compounds. Vitamin K denotes a group of lipophilic and hydrophobic vitamins that are needed for the post-translational modification of certain proteins, mostly required for blood coagulation. Chemically they are 2-methyl-1,4-naphthoquinone derivatives.Vitamin K is not a single compound, rather it is a series of related analogues. Vitamin K1 is called phylloquinone and has the systematic name all-E-2-methyl-3-(3,7,11,15-tetramethylhexadec-2-enyl)naphthalene-1,4-dione. Vitamin K2 (menaquinone) is normally produced by bacteria in the intestines, and dietary deficiency is extremely rare unless the intestines are heavily damaged or are unable to absorb the molecule.Vitamin K2 is a ...

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28-07-2016 дата публикации

COMPOSITION CONTAINING REDUCED COENZYME Q10 AND PRODUCTION METHOD THEREOF

Номер: US20160214919A1
Принадлежит: KANEKA CORPORATION

The present invention provides a particulate composition wherein an oil component containing reduced coenzyme Qis polydispersed forming a domain in a matrix containing a water-soluble excipient, which simultaneously shows high oxidative stability and high oral absorbability, a production method thereof, and a stabilizing method thereof. It also provides a food, food with nutrient function claims, food for specified health uses, dietary supplement, nutritional product, animal drug, drink, feed, pet food, cosmetic, pharmaceutical product, therapeutic drug, prophylactic drug and the like, which contain the composition. 121-. (canceled)22. A method of producing a particulate composition comprising reduced coenzyme Q , which comprises suspending a oil-in-water emulsion composition prepared from an oil component (A) containing reduced coenzyme Qand an aqueous solution containing a water-soluble excipient in oil component (B) , and removing water from the emulsion composition in oil component (B).23. The production method of claim 22 , wherein the oil component (B) comprises 5-100 wt % of fat and oil and 0-95 wt % of surfactant (E).24. The production method of claim 22 , wherein the oil component (B) comprises 5-99.99 wt % of fat and oil and 0.01-95 wt % of surfactant (E).25. The production method of claim 23 , wherein the surfactant (E) is at least one kind selected from the group consisting of glycerol fatty acid ester claim 23 , polyglycerin ester claim 23 , sucrose fatty acid ester claim 23 , sorbitan fatty acid ester and polyoxyethylenesorbitan fatty acid ester claim 23 , each having an HLB of not more than 10 claim 23 , and lecithins.26. A method of producing a particulate composition comprising reduced coenzyme Q claim 23 , which comprises spray drying claim 23 , in a gaseous phase claim 23 , an oil-in-water emulsion composition prepared from an oil component (A) comprising reduced coenzyme Qand an aqueous solution comprising a water-soluble excipient.27. The ...

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02-08-2018 дата публикации

PREPARATION OF 2,6- AND 2,7-DISUBSTITUTED ANTHRAQUINONE DERIVATES

Номер: US20180215694A1
Принадлежит: BASF SE

A composition comprising a compound of formula (Va) wherein n is 1 or 2 and wherein m is 1 or 2, with n and m preferably both being 1 or both being 2, more preferably both being 1, and/or, preferably and, a compound of formula, wherein n is 1 or 2 and wherein m is 1 or 2, with n and m preferably both being 1 or both being 2, more preferably both being 1, and wherein at least 90 weight-% of the composition consist of compounds of formula (Va) and formula (Vb). 2: The process of claim 1 , whereinthe mixture (A) provided in (i) comprises a compound of formula (II) wherein x is 1 and the mixture (B) obtained in (ii) comprises a compound of formula (IIIa) and a compound of formula (IIIb) wherein n is 1 and m is 1, and the mixture (C) obtained in (iii) comprises a compound of formula (IVa) and a compound of formula (IVb) wherein n is 1 and m is 1; orwherein the mixture (A) provided in (i) comprises a compound of formula (II) wherein x is 2 and the mixture (B) obtained in (ii) comprises a compound of formula (IIIa) and a compound of formula (IIIb) wherein n is 2 and m is 2, and the mixture (C) obtained in (iii) comprises a compound of formula (IVa) and a compound of formula (IVb) wherein n is 2 and m is 2.3: The process of claim 1 , wherein the sequence of (i) to (iii) is carried out as a one-pot process.4: The process of claim 1 , wherein the dehydrogenation catalyst according to (i) comprises at least one element selected from the group consisting of palladium claim 1 , platinum claim 1 , copper claim 1 , lithium claim 1 , zinc claim 1 , zirconium claim 1 , and aluminum.5: The process of claim 1 , wherein said providing the mixture (a) according to (I) comprises admixing the compound of formula (I) with the compound of formula (ii) at a molar ratio of the compound of formula (I) relative to the compound of formula (ii) in the range of from 0.1:1 to 0.5:1.6: The process of claim 1 , wherein the liquid solvent system according to (i) comprises at least one organic solvent ...

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10-08-2017 дата публикации

ELECTROCHEMICALLY ACTIVE AGENTS FOR PH MODULATION IN BIOLOGICAL BUFFERS

Номер: US20170226037A1
Принадлежит:

Device and methods for use in a biosensor comprising a multisite array of test sites, the device and methods being useful for modulating the binding interactions between a (biomolecular) probe or detection agent and an analyte of interest by modulating the pH or ionic gradient near the electrodes in such biosensor. An electrochemically active agent that is suitable for use in biological buffers for changing the pH of the biological buffers. Method for changing the pH of biological buffers using the electrochemically active agents. The methods of modulating the binding interactions provided in a biosensor, analytic methods for more accurately controlling and measuring the pH or ionic gradient near the electrodes in such biosensor, and analytic methods for more accurately measuring an analyte of interest in a biological sample. 1. A method comprising: the quinone derivative has a reduced reactivity with a nucleophile compared to a reactivity between the quinone and the nucleophile;', {'sub': n', '2n+1', '2', 'n', '2n', 'n', '2n', 'n', '2n', 'y', 'n', '2n', 'y', 'n', '2n+1', 'n', '2n', 'y', 'n', '2n', 'y', 'n', '2n+1', 'n', '2n+1', 'n', '2n+1', '2', '3', '3', '2', 'n', '2n+1', 'n', '2n+1', '2', 'n', '2n', 'n', '2n', '2', 'n', '2n', '2', 'n', '2n', '2', 'n', '2n+1', 'n', '2n+1', 'n', '2n+1', 'n', '2n+1', 'n', '2n', 'n', '2n+1', 'n', '2n', '2', 'n', '2n+1', 'n', '2n', 'n', '2n', 'n', '2n', 'n', '2n', 'y', 'n', '2n', 'y', 'n', '2n+1', 'n', '2n', 'y', 'n', '2n', 'y', 'n', '2n', 'n', '2n', 'y', 'n', '2n', 'y', 'n', '2n+1', 'n', '2n', 'n', '2n', 'n', '2n', 'n', '2n', 'n', '2n', 'n', '2n', 'n', '2n', 'n', '2n', 'n', '2n+1', 'n', '2n', 'n', '2n+1', 'n', '2n+1', 'n', '2n+1', 'n', '2n', 'n', '2n+1', 'n', '2n', 'n', '2n+1', 'n', '2n', 'y', 'n', '2n+1', '2', '2n', 'y', 'n', '2n+1', '2', '2n+1', 'n', '2n+1', 'n', '2n+1', 'n', '2n+1', 'n', '2n+1', 'n', '2n+1', 'n', '2n+1', '2', 'n', '2n+1', '3', 'n', '2n+1', '3', 'n', '2n+1', '2', 'n', '2n+1', 'n', '2n+1', 'n', '2n+1', 'n', '2n+1', ...

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23-07-2020 дата публикации

ERASING UNIT AND ERASING METHOD

Номер: US20200230992A1
Принадлежит:

An erasing unit according to an embodiment of the present disclosure is a unit that performs erasing of information written on a reversible recording medium. This erasing unit includes: a light source section including one or a plurality of laser devices; and a controller that controls the light source section to cause the light source section to emit a smaller number of laser light beams having emission wavelengths than the number of the recording layers included in the reversible recording medium. 1. An erasing unit , the erasing unit that performs erasing of information written on a reversible recording medium , the reversible recording medium including recording layers and heat-insulating layers alternately stacked , the recording layers each including a reversible heat-sensitive color developing composition and a photothermal conversion agent , developing colors of the respective reversible heat-sensitive color developing compositions differing among the recording layers , absorption wavelengths of the respective photothermal conversion agents differing among the recording layers , the erasing unit comprising:a light source section including one or a plurality of laser devices; anda controller that controls the light source section to cause the light source section to apply, to the reversible recording medium, a smaller number of laser light beams having emission wavelengths than a number of the recording layers included in the reversible recording medium.2. The erasing unit according to claim 1 , further comprising a receiving section that receives an input of a first identifier that identifies a type of the reversible recording medium claim 1 ,wherein the controller controls the light source section to cause the light source section to apply, to the reversible recording medium, a smaller number of laser light beams having emission wavelengths than a number of the recording layers included in the reversible recording medium corresponding to the first ...

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27-11-2014 дата публикации

Production of Glutaric Acid and Derivatives from Carbohydrate-Containing Materials

Номер: US20140350297A1
Принадлежит: Rennovia, Inc.

The present invention generally relates to processes for the chemocatalytic conversion of a pentose source to a glutaric acid product. The present invention includes processes for the conversion of pentose to a glutaric acid product via pentaric acid or derivatives thereof. The present invention also includes processes comprising the catalytic oxidation of pentose to pentaric acid and catalytic hydrodeoxygenation of pentaric acid or derivatives thereof to a glutaric acid product. 151-. (canceled)53. The process of wherein X is hydroxyl and Ris independently a salt-forming ion claim 52 , hydrogen claim 52 , hydrocarbyl claim 52 , or substituted hydrocarbyl.54. The process of wherein the C5-backbone substrate comprises a pentaric acid.55. The process of wherein the pentaric acid comprises an acid selected from the group consisting of xylaric acid claim 54 , arabinaric acid claim 54 , and ribaric acid.56. The process of wherein C5-backbone substrate comprises xylaric acid.57. The process of wherein the heterogeneous oxidation catalyst comprises a metal selected from the group consisting of Pd claim 52 , Pt claim 52 , and combinations thereof.58. The process of wherein the heterogeneous oxidation catalyst comprises Pt.59. The process of wherein the weight ratio of pentose to Pd and/or Pt is no greater than about 65:1.60. The process of wherein the metal constitutes from about 0.25% to about 10% of the total weight of the catalyst.61. The process of wherein the metal constitutes from about 1% to about 8% of the total weight of the catalyst.62. The process of wherein the heterogeneous oxidation catalyst comprises a catalyst support selected from the group consisting of carbon claim 52 , alumina claim 52 , silica claim 52 , titania claim 52 , zirconia claim 52 , and zeolite.63. The process of wherein the pH of the reaction mixture is less than 6.64. The process of wherein the reaction is conducted in the substantial absence of added base.65. The process of wherein the ...

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14-09-2017 дата публикации

Method of Making Vitamin K1

Номер: US20170260117A1
Принадлежит: Sunny Pharmtech Inc.

This invention discloses a method of making vitamin K1. The mentioned method of making vitamin K1 comprises performing a first one-pot synthesis with base catalyst, performing a first hydrolysis, performing a substitution, and performing a second one-pot synthesis without metal oxidant. The starting material of this invention is stable 2-methyl-1,4-naphthoquinone. Preferably, this invention provides a method of making vitamin K1 efficiently on simplifying the operation and decreasing the side-product. More preferably, without metal residue, the vitamin K1 of this invention is without metal residue and more safety for clinical application. 1. A method of making vitamin K1 , comprising:performing a first one-pot synthesis to produce 2-methyl-1,4-naphthohydroquinone di-alkyl ester from 2-methyl-1,4-naphthoquinone with a base catalyst, wherein said first one-pot synthesis includes a hydrogenation in situ esterification procedure;performing a first hydrolysis procedure with an organic base to produce 2-methyl-1,4-naphthohydroquinone mono-alkyl ester from the 2-methyl-1,4-naphthohydroquinone di-alkyl ester;performing a substitution procedure to generate 2-methyl-3-phytyl-1,4-naphthohydroquinone mono-alkyl ester from the 2-methyl-1,4-naphthohydroquinone mono-alkyl ester; andperforming a second one-pot synthesis to form vitamin K1 from 2-methyl-3-phytyl-1,4-naphthohydroquinone mono-alkyl ester, wherein said second one-pot synthesis includes a second hydrolysis procedure and an oxidation procedure.2. The method of making vitamin K1 according to claim 1 , wherein said base catalyst in said one-pot synthesis is amine.3. The method of making vitamin K1 according to claim 1 , wherein said base catalyst is selected from one of the group consisting of the following: 4-dimethylaminopyridine (DMAP) claim 1 , triethylamine (TEA) claim 1 , 4-methyl-morpholine claim 1 , dimethylaniline claim 1 , methyl nicotinate claim 1 , imidazole claim 1 , pyridine claim 1 , methyl pyridine.4. The ...

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14-10-2021 дата публикации

PROCESS OF VITAMIN K2 DERIVATIVES PREPARATION

Номер: US20210317060A1
Принадлежит:

Provided is an improved process of vitamin K2 derivatives preparation, represented by formula (I) wherein n is an integer from 3 to 13. 2. The process according to claim 1 , characterized in that the α-sulfonyl carbanion is generated by means of an alkali metal hexamethyldisilazyde claim 1 , preferably sodium hexamethyldisilazyde claim 1 , in a polar aprotic solvent claim 1 , such as tetrahydrofuran claim 1 , dimethylformamide claim 1 , heksamethylophosphoramide or the mixture thereof.3. The process according to any of the preceding claims claim 1 , characterized in that phenylsulfonyl groups are removed with sodium amalgam in MeOH claim 1 , buffered with NaHPO.4. The process according to any of the preceding claims claim 1 , characterized in that the oxidative deallylation is accomplished with the use of Pd(OAc)/PhP and 1 claim 1 ,3-dimethylbarbituric acid.8. The process according to any of the preceding claims claim 1 , characterized in that the MK-7 type of vitamin K2 is obtained.11. The process according to claim 10 , characterized in that NaCOor KCOis used as the solid inorganic base. The present invention relates to the process of vitamin Kderivatives preparation.Vitamins Kplay an important role in the blood coagulation cascade and bones supplementation. Synthetic vitamins Kcould be used as the active ingredients of the drug products as well in the dietary supplements.Vitamins K, called menaquinones (MK-n) or pharnoquinones, are characterized by the menadione structure with a polyprenyl side chain at C-3 position consisting of a different number of isoprene units in the side chain (n=1-13). They are represented by the formula depicted below:Different biological activity and bioavailability of menaquinones result from the chain length and the number of unsaturated bonds present in that side chain [2007, 43(3), 277-281].Vitamin K, as a cofactor of γ-carboxylase, is involved in posttraslational γ-carboxylation of certain glutamate residues in precursor proteins ...

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29-10-2015 дата публикации

PROCESS FOR THE PREPARATION OF A STABLE POLYMORPHIC FORM OF ATOVAQUONE

Номер: US20150307431A1
Принадлежит: TARO PHARMACEUTICAL INDUSTRIES LIMITED

The present invention provides a process for the preparation of a stable polymorph III of Atovaquone exhibiting characteristic peaks (expressed in degrees 20±0.2°θ) at about 6.9, 9.6, 14.1, 14.7, 17.0, 18.5, 19.1, 19.9, 20.3, 22.0, 22.6, 23.2, 24.2, 26.8, and 28.5, which comprises: (a) providing a sample of Atovaquone particles; (b) heating the sample of Atovaquone particles at a minimal temperature of between 140° C. to 160° C. depending on the particle size of the sample; and (c) cooling the sample to obtain the stable polymorphic form of Atovaquone. 1. A process for the preparation of a stable polymorph III of Atovaquone which comprises:(a) providing a sample of Atovaquone particles;(b) heating the sample of Atovaquone particles of step (a) at a temperature of at least about 160° C. for a time sufficient of at least about one hour to obtain a stable polymorphic form of Atovaquone, having characteristic peaks (expressed in degrees 20±0.2° θ) at approximately one or more of the positions: about 6.9, 9.6, 14.1, 14.7, 17.0, 18.5, 19.1, 19.9, 20.3, 22.0, 22.6, 23.2, 24.2, 26.8, and 28.5; and(c) cooling the sample of step (b).2. A process for the preparation of a stable polymorph III of Atovaquone which comprises:(a) providing a sample of Atovaquone particles wherein at least about 90% of the Atovaquone particles have a volume diameter of equal or less than about 40μ;(b) heating the sample of Atovaquone particles of step (a) at a temperature of at least about 140° C. for a time sufficient to obtain a stable polymorphic form of Atovaquone, having characteristic peaks (expressed in degrees 20±0.2° θ) at approximately one or more of the positions about 6.9, 9.6, 14.1, 14.7, 17.0, 18.5, 19.1, 19.9, 20.3, 22.0, 22.6, 23.2, 24.2, 26.8, and 28.5; and(c) cooling the sample of step (b).3. The process of claim 1 , wherein the Atovaquone particles of step (c) are further micronized if non-micronized particles are used in step (a) claim 1 , to obtain Atovaquone particles having ...

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19-10-2017 дата публикации

METHODS FOR SELECTIVE OXIDATION OF ALPHA TOCOTRIENOL IN THE PRESENCE OF NON-ALPHA TOCOTRIENOLS

Номер: US20170297991A1
Автор: MOLLARD Paul
Принадлежит:

A method of producing alpha-tocotrienol quinone or a stereoisomer thereof, the method comprising selective opening of alpha-tocotrienol chroman to alpha-tocotrienol quinone in the presence of non-alpha tocotrienol chromans by oxidizing alpha-tocotrienol with a metal salt oxidizing agent, wherein the stoichiometric ratio of metal salt oxidizing agent/alpha-tocotrienol is at least 4:1 and wherein said metal oxidizing agent is added in sequential additions, in order to reduce oxidation of any amounts of non-alpha tocotrienol chromans that might have been present in the starting alpha-tocotrienol chroman material. This process uses conditions favoring oxidation rates of the alpha tocotrienol chroman vs. the non-alpha tocotrienol chromans. 2. The method according to comprising oxidizing alpha-tocotrienol with a metal salt oxidizing agent claim 1 , in a biphasic solution claim 1 , wherein the alpha-tocotrienol is dissolved in a non-polar solvent; the metal salt oxidizing agent is dissolved in a polar solvent; and the separate solutions are mixed to permit the oxidation.3. The method according to or claim 1 , wherein the metal salt oxidizing agent is an iron(III) salt selected from an iron(III) halide claim 1 , an iron(III) acetate claim 1 , an iron(III) citrate claim 1 , an iron(III) nitrate claim 1 , iron(III) tartrate or an iron(III) phosphate.4. The method according to or claim 1 , wherein the metal salt oxidizing agent is iron chloride (Fe(III)Cl).5. The method according to claim 4 , wherein the metal oxidizing agent is sufficient to oxidize at least about 98% of the alpha-tocotrienol chroman into the alpha-tocotrienol quinone.6. The method according to claim 5 , wherein the composition resulting from the oxidation has less than about 1% of one or more non-alpha-tocotrienol quinone compounds selected from alpha-tocotrienol claim 5 , beta-tocotrienol claim 5 , beta-tocotrienol quinone claim 5 , gamma-tocotrienol claim 5 , gamma-tocotrienol quinone claim 5 , delta- ...

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26-11-2015 дата публикации

PROCESS FOR PREPARING 2,2'-BIPHENOLS USING SELENIUM DIOXIDE

Номер: US20150336865A1
Принадлежит: EVONIK DEGUSSA GmbH

A process for preparing a 2,2′-biphenol, proceeds by a) adding a first phenol to a reaction mixture, b) adding a second phenol to the reaction mixture, c) adding selenium dioxide to the reaction mixture, d) adding an acid having a pKa in the range from 0.0 to 5.0 to the reaction mixture, and e) heating the reaction mixture such that the first phenol and the second phenol are converted to said 2,2′-biphenol. 1. A process for preparing a 2 ,2′-biphenol , comprising:a) adding a first phenol to a reaction mixture,b) adding a second phenol to the reaction mixture,c) adding selenium dioxide to the reaction mixture,d) adding an acid having a pKa in the range from 0.0 to 5.0 to the reaction mixture, ande) heating the reaction mixture such that the first phenol and the second phenol are converted to said 2,2′-biphenol.3. The process according to claim 2 , wherein R claim 2 , R claim 2 , R claim 2 , R claim 2 , Rare each independently selected from the group consisting of:{'sub': 1', '12', '1', '12', '6', '20', '6', '20, '—H, —(C-C)-alkyl, —O—(C-C)-alkyl, —(C-C)-aryl, and —O—(C-C)-aryl,'}wherein the alkyl and aryl groups mentioned are optionally substituted, and{'sup': 1', '5, 'wherein at least Ror Ris —H.'}4. The process according to claim 2 , wherein R claim 2 , R claim 2 , Rare each independently selected from the group consisting of:{'sub': 1', '12, '—H, and —(C-C)-alkyl,'}wherein the alkyl groups mentioned are optionally substituted, and{'sup': 1', '5, 'wherein at least Ror Ris —H.'}6. The process according to claim 5 , wherein R claim 5 , R claim 5 , R claim 5 , R claim 5 , Rare each independently selected from the group consisting of:{'sub': 1', '12', '1', '12', '6', '20', '6', '20, '—H, —(C-C)-alkyl, —O—(C-C)-alkyl, —(C-C)-aryl, and —O—(C-C)-aryl,'}wherein the alkyl and aryl groups mentioned are optionally substituted, and{'sup': 6', '10, 'wherein at least Ror Ris —H.'}7. The process according to claim 5 , wherein R claim 5 , R claim 5 , Rare each independently ...

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08-11-2018 дата публикации

METHODS FOR SELECTIVE OXIDATION OF ALPHA TOCOTRIENOL IN THE PRESENCE OF NON-ALPHA TOCOTRIENOLS

Номер: US20180319730A1
Автор: MOLLARD Paul
Принадлежит: BioElectron Technology Corporation

A method of producing alpha-tocotrienol quinone or a stereoisomer thereof, the method comprising selective opening of alpha-tocotrienol chroman to alpha-tocotrienol quinone in the presence of non-alpha tocotrienol chromans by oxidizing alpha-to-cotrienol with a metal salt oxidizing agent, wherein the stoichiometric ratio of metal salt oxidizing agent/alpha-tocotrienol is at least 4:1 and wherein said metal oxidizing agent is added in sequential additions, in order to reduce oxidation of any amounts of non-alpha tocotrienol chromans that might have been present in the starting alpha-tocotrienol chroman material. This process uses conditions favoring oxidation rates of the alpha tocotrienol chroman vs. the non-alpha tocotrienol chromans. 115.-. (canceled)17. The method according to comprising oxidizing alpha-tocotrienol with the metal salt oxidizing agent in a biphasic solution claim 16 , wherein a first solution comprises the alpha-tocotrienol dissolved in a non-polar solvent; a second solution comprises the metal salt oxidizing agent dissolved in a polar solvent; and the separate first and second solutions are mixed to permit the oxidation.18. The method according to claim 16 , wherein the metal salt oxidizing agent is sufficient to oxidize at least about 98% of the alpha-tocotrienol into the alpha-tocotrienol quinone.19. The method according to claim 18 , wherein the composition resulting from the oxidation has less than about 1% of one or more compounds selected from the group consisting of alpha-tocotrienol claim 18 , beta-tocotrienol claim 18 , beta-tocotrienol quinone claim 18 , gamma-tocotrienol claim 18 , gamma-tocotrienol quinone claim 18 , delta-tocotrienol claim 18 , delta-tocotrienol quinone claim 18 , and combinations thereof.20. The method according to claim 18 , wherein the composition resulting from the oxidation has less than about 0.7% of one or more compounds selected from the group consisting of alpha-tocotrienol claim 18 , beta-tocotrienol claim ...

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15-10-2020 дата публикации

NON-CONTACT THERMAL PRINTING OF COLOR THERMOCHROMIC MATERIALS

Номер: US20200324565A1
Принадлежит:

A system includes an unpatterned heater configured to pre-heat a thermochromic coating disposed on a substrate to a first temperature. The thermochromic coating has a threshold temperature at which the thermochromic material undergoes a color change. The system also includes a patterned heater comprising multiple heating elements configured to heat selected pixels of the thermochromic coating to a temperature at or above the threshold temperature according to a predetermined pattern. An air gap is maintained between the multiple heating elements and the thermochromic material while the patterned heater is heating the thermochromic material. The air in the air gap heated to a second temperature. 1. A system comprising:an unpatterned heater configured to pre-heat a thermochromic coating disposed on a substrate to a first temperature, the thermochromic coating having a threshold temperature at which the thermochromic material undergoes a color change;a patterned heater comprising multiple heating elements configured to heat selected pixels of the thermochromic coating to a temperature at or above the threshold temperature according to a predetermined pattern; andan air gap maintained between the multiple heating elements and the thermochromic material while the patterned heater is heating the thermochromic material, air in the air gap heated to a second temperature.2. The system of claim 1 , further comprising a movement mechanism configured to move the substrate having the thermochromic material disposed thereon relative to the multiple heating elements.3. The system of claim 2 , wherein each heating element is suspended on a flexure arm that floats above the thermochromic material.4. The system of claim 1 , wherein the gap is between about 5 μm and 20 μm.5. The system of claim 1 , wherein the air is heated by the unpatterned heater.6. The system of claim 1 , wherein the unpatterned heater comprises one or more of a rotating heated drum claim 1 , an infrared heater ...

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17-12-2015 дата публикации

METHODS FOR THE VALORIZATION OF CARBOHYDRATES

Номер: US20150361022A1
Принадлежит:

There are provided methods for the valorization of carbohydrates. The methods comprise reacting a fluid comprising at least one carbohydrate with at least one metal catalyst or at least one metal catalytic system in a fluidized bed reactor so as to obtain at least one organic acid or a derivative thereof. 1. A method for the valorization of carbohydrates , said method comprising:reacting a fluid comprising at least one carbohydrate with at least one oxidation metal catalyst or at least one oxidation metal catalytic system in a fluidized bed reactor so as to obtain at least one organic acid or an anhydride thereof, a salt thereof, an amide thereof, an ester thereof or an acid halide,said at least one oxidation metal catalyst or said at least one oxidation metal catalytic system comprising at least one metal chosen from V, Au, Cr, Mg, Ag, Pt, Rh, Sn, Al, Ce, Ru, Mo, Re, Pd, Te, Ta, Si, Sb, Nb, Cu, Zr, Ti, Mn, Zn, W, Ni and Fe.2. The method of claim 1 , wherein said method comprises injecting atomized droplets of a carbohydrate-containing composition that comprises said at least one carbohydrate and water into said fluidized bed reactor.3. The method of claim 2 , wherein said atomized droplets are vaporized in situ when inserted into said fluidized bed reactor.4. The method of claim 3 , wherein said carbohydrate is at a concentration of about 1 wt % to about 20 wt % claim 3 , based on the total weight of the carbohydrate-containing composition.5. The method of claim 2 , wherein said carbohydrate is at a concentration of about 5 wt % to about 15 wt % claim 2 , based on the total weight of the carbohydrate-containing composition.6. The method of claim 5 , wherein said composition is injected at a rate of about 0.5 mL/minute to about 10 mL/minute per about 0.2 L of capacity of said fluidized bed reactor.7. The method of claim 1 , wherein said method involves the use of said at least one oxidation metal catalyst that is chosen from vanadium pyrophosphate claim 1 , iron ...

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22-12-2016 дата публикации

METHOD FOR PRODUCING 2,3,5-TRIMETHYL BENZOQUINONE BY OXIDATION OF 2,3,6-TRIMETHYLPHENOL

Номер: US20160368887A1
Принадлежит:

The invention relates to a method for producing 2,3,5-trimethyl benzoquinone or a compound containing 2,3,5-trimethyl benzoquinone, the method comprising the following steps: Oxidation of 2,3,6-trimethylphenol with oxygen or an oxygen-containing gas in a two-or multi-phase reaction medium in the presence of a catalyst or catalyst system containing at least one copper (II)-halide to a mixture containing 2,3,5-trimethyl benzoquinone, characterized in that the reaction medium contains water and at least one secondary aliphatic acyclic alcohol having 6 or more, preferably 7 or more, carbon atoms. 115.-. (canceled)16. A process for preparing 2 ,3 ,5-trimethylbenzoquinone or a mixture comprising 2 ,3 ,5-trimethylbenzoquinone , comprising the following step:(i) oxidizing 2,3,6-trimethylphenol to 2,3,5-trimethylbenzoquinone with oxygen or an oxygen-containing gas in a two-phase or multiphase reaction medium in the presence of a catalyst or catalyst system at least comprising a copper(II) halide, to give a mixture comprising 2,3,5-trimethylbenzoquinone,wherein the reaction medium comprises water and at least one secondary aliphatic acyclic alcohol having 6 or more carbon atoms.17. The process according to claim 16 , wherein said at least one secondary aliphatic acyclic alcohol having 7 or more carbon atoms18. The process according to claim 16 , wherein the catalyst or the catalyst system comprises copper (II) chloride.19. The process according to claim 16 , wherein the catalyst or the catalyst system further comprises at least one alkali metal halide.20. The process according to claim 19 , wherein said at least one alkali metal halide is lithium chloride.21. The process according to claim 16 , wherein the reaction medium comprises 3-heptanol.22. The process according to claim 16 , wherein the process is carried out batchwise.23. The process according to claim 16 , wherein the mixture comprising 2 claim 16 ,3 claim 16 ,5-trimethylbenzoquinone is washed in a step (ii) with an ...

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20-12-2018 дата публикации

METHOD OF FORMING PHENYLENE ETHER OLIGOMER

Номер: US20180362430A1
Принадлежит: SABIC Global Technologies

A phenylene ether oligomer is prepared by a process that includes partially converting 2,6-dimethylphenol to 3,3′,5,5′-tetramethyl-4,4′-dihydroxybiphenyl and/or 3,3′,5,5′-tetramethyldiphenoquinone, converting the residual 2,6 dimethylphenol to poly(2,6-dimethyl-1,4-phenylene ether) and any 3,3′,5,5′-tetramethyl-4,4′-dihydroxybiphenyl to 3,3′,5,5′-tetramethyldiphenoquinone, and reacting the poly(2,6-dimethyl-1,4-phenylene ether) and 3,3′,5,5′-tetramethyldiphenoquinone to form the phenylene ether oligomer. The preparation can be conducted without isolation of intermediates. 2. The method of claim 1 , wherein the alkylenediamine is selected from the group consisting of N claim 1 ,N′-di-(C-alkyl)ethylenediamines claim 1 , N claim 1 ,N claim 1 ,N′-tri-(C-alkyl)ethylenediamines claim 1 , N claim 1 ,N claim 1 ,N′N′-tetra-(C-alkyl)ethylenediamines claim 1 , N claim 1 ,N′-di-(C-alkyl)-1 claim 1 ,2-propylenediamines claim 1 , N claim 1 ,N claim 1 ,N′-tri-(C-alkyl)-1 claim 1 ,2-propylenediamines claim 1 , N claim 1 ,N claim 1 ,N′N′-tetra-(C-alkyl)-1 claim 1 ,2-propylenediamines claim 1 , N claim 1 ,N′-di-(C-alkyl)-1 claim 1 ,3-propylenediamines claim 1 , N claim 1 ,N claim 1 ,N′-tri-(C-alkyl)-1 claim 1 ,3-propylenediamines claim 1 , N claim 1 ,N claim 1 ,N′N′-tetra-(C-alkyl)-1 claim 1 ,3-propylenediamines claim 1 , and combinations thereof.3. The method of or claim 1 , wherein the alkylenediamine is selected from the group consisting of N claim 1 ,N′-di-tert-butylethylenediamine claim 1 , N claim 1 ,N claim 1 ,N′ claim 1 ,N′-tetraethylethylenediamine claim 1 , N claim 1 ,N claim 1 ,N′ claim 1 ,N′-tetramethylethylenediamine claim 1 , N claim 1 ,N′-diethyl-N claim 1 ,N′-dimethylethylenediamine claim 1 , N claim 1 ,N′-diethylethylenediamine claim 1 , N claim 1 ,N′-dimethylethylenediamine claim 1 , N claim 1 ,N claim 1 ,N′ claim 1 ,N′-tetramethyl-1 claim 1 ,3-butylenediamine claim 1 , and combinations thereof.4. The method of any one of - claim 1 , wherein the reaction of the 2 ...

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05-12-2019 дата публикации

DEUTERATED IDEBENONE

Номер: US20190367438A1
Автор: Tung Roger D.
Принадлежит:

The present invention in one embodiment provides a compound of Formula I: 123-. (canceled)25. The method of claim 24 , wherein in the compound of Formula I claim 24 , Ris CH.26. The method of claim 24 , wherein in the compound of Formula I claim 24 , Ris CD.27. The method of claim 24 , wherein in the compound of Formula I claim 24 , Ris CH.28. The method of claim 24 , wherein in the compound of Formula I claim 24 , Ris CD.29. The method of claim 24 , wherein in the compound of Formula I claim 24 , Ris CH.30. The method of claim 24 , wherein in the compound of Formula I claim 24 , Ris CD.31. The method of claim 24 , wherein in the compound of Formula I claim 24 , each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; each Yis deuterium; and each Yis deuterium.35. The method of claim 24 , wherein in the compound of Formula I claim 24 , the deuterium incorporation at each designated deuterium atom is at least 90%.36. The method of claim 24 , wherein the deuterium incorporation at each designated deuterium atom is at least 95%. This application is a continuation of U.S. application Ser. No. 16/008,676, filed on Jun. 14, 2018, which is a continuation of U.S. application Ser. No. 14/414,039 (now U.S. Pat. No. 10,017,445), filed on Jan. 9, 2015, which is the U.S. National Stage of International Application No. PCT/US2013/050302, filed on Jul. 12, 2013, published in English, which claims the benefit of U.S. Provisional Application No. 61/670,716, filed on Jul. 12, 2012. The entire teachings of the above application(s) are incorporated herein by reference.Many current medicines suffer from poor absorption, distribution, metabolism and/or excretion (ADME) properties that prevent their wider use or limit their use in certain indications. Poor ADME properties are also a major reason for the failure of drug candidates in clinical trials. While formulation technologies and prodrug strategies can be employed in some cases to improve ...

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31-12-2020 дата публикации

Quinones and process of obtaining same

Номер: US20200407303A1
Принадлежит: BASF SE

Disclosed is a process for the oxidation of at least one chroman (C1) in a solvent mixture comprising at least two solvents or in a C-bearing solvent, with a gaseous compound comprising, essentially consisting of, or consisting of oxygen in the presence of a copper catalyst, said copper catalyst exhibiting the oxidation state (+1) or (+2). A further part of the disclosure is a composition comprising at least one chroman (C1) and/or at least one quinone (C30), a solvent mixture comprising at least two solvents or a C-bearing solvent, a copper catalyst, said copper catalyst exhibiting the oxidation state (+1) or (+2) and a gaseous compound comprising, essentially consisting or consisting of oxygen. A quinone preparation and a process of making same is also part of the invention.

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17-04-2001 дата публикации

Methods of recovering catalyst in solution in the oxidation of cyclohexane to adipic acid

Номер: US6218573B1
Принадлежит: RPC Inc

This invention relates to methods of controlling the oxidation of cyclohexane to adipic acid in the presence of a monobasic acid solvent, by removing the catalyst from the reaction mixture, outside the reaction zone. Substantially all the unreacted cyclohexane along with at least the majority of the monobasic acid solvent are removed. A substantially non-solvent for the catalyst (first constituent), and water are added into the resulting mixture, in such amounts as to maintain one solids-free single liquid phase. This process is highly facilitated in the presence of considerable amounts of adipic acid. The catalyst may then be extracted with water from the solids-free single liquid phase. A water phase containing dissolved catalyst may also be formed by addition of small amounts of a solvent which is substantially non-solvent for the catalyst and substantially non-solvent for the dibasic acids (second constituent), and/or dropping the temperature. Adipic acid may be precipitated after catalyst removal with further addition of second constituent and/or dropping the temperature.

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09-07-2002 дата публикации

Methods and replacing water and cyclohexanone with acetic acid in aqueous solutions of catalyst

Номер: US6417128B1
Принадлежит: RPC Inc

This invention relates to methods of replacing water and cyclohexanone with acetic acid in an aqueous solution of catalyst, preferably a cobalt compound. Such an aqueous solution is produced by extracting catalyst with water from a cyclohexanone/water solution of reaction products made by the direct oxidation of cyclohexane to adipic acid. The replacement of both water and cyclohexanone are conducted in a solvent exchange column, wherein acetic acid dissolves the catalyst, while water vapors force the cyclohexanone into a condenser, followed by a decanter wherein two liquid phases may be formed and separated; an upper liquid phase containing a majority of cyclohexanone and a lower liquid phase containing a majority of water. The cyclohexanone may be removed in a pretreatment zone, wherein also part of the water may be removed, before the concentrated catalyst extract enters the solvent exchange column.

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13-08-2002 дата публикации

Methods of extracting catalyst from a reaction mixture in the oxidation of cyclohexane to adipic acid

Номер: US6433220B1
Принадлежит: RPC Inc

This invention relates to methods of controlling the oxidation of cyclohexane to adipic acid in the presence of a monobasic acid solvent, by extracting the catalyst from the reaction mixture, outside the reaction zone. Substantially all the unreacted cyclohexane, the majority of adipic acid, and preferably substantially all the monobasic acid solvent are removed from the reaction product. In the case that substantially all the monobasic acid solvent is removed, protic solvent, is added intermittently or continuously in the reaction mixture during the removal of the monobasic acid solvent, preferably by distillation, thus preventing solids precipitation. Dipolar aprotic solvent is then added in the presence of an adequate amount of the protic solvent (the total of dipolar aprotic solvent and the protic solvent constituting a novel combination solvent) to maintain a single liquid phase, followed by a step of extracting substantially all the catalyst in protic solvent. The catalyst extract is preferably recycled to the reaction zone, where the cyclohexane is oxidized to adipic acid. Thus, the novel combination solvent, which is preferably a combination of cyclohexanone with water, allows the dissolution of the reaction product, preferably after removal of the majority of the adipic acid, followed by a substantially complete extraction of the catalyst in water. No catalyst precipitation takes place, and all disadvantages and costs of solids handling are prevented.

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13-08-2002 дата публикации

Methods of separating catalyst in solution from a reaction mixture produced by oxidation of cyclohexane to adipic acid

Номер: US6433221B1
Принадлежит: RPC Inc

This invention relates to methods of controlling the oxidation of cyclohexane to adipic acid in the presence of a monobasic acid solvent, by separating the catalyst from the reaction mixture, outside the reaction zone. Substantially all the unreacted cyclohexane, the majority of adipic acid, and substantially all the monobasic acid solvent are preferably removed. A protic solvent, may be added intermittently or continuously in the reaction mixture during the removal of the monobasic acid solvent, preferably by distillation, for preventing solids precipitation. A dipolar aprotic solvent is then added in the presence of an adequate amount of the protic solvent to maintain a single liquid phase, followed by a step of formation of two liquid phases, a solids-free protic liquid phase containing substantially all the catalyst, and a solids-free aprotic liquid phase containing at least the majority of ingredients of the reaction mixture. The formation of the two phases is performed by a process selected from a group consisting of lowering the first temperature to a second temperature, adding additional protic solvent, adding an apolar aprotic solvent, and a combination thereof.

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11-05-2021 дата публикации

环己烷直接氧化制己二酸的自由基保护剂

Номер: CN109096096B
Автор: 唐泓, 干丰丰

本发明涉及环己烷直接氧化制己二酸的自由基保护剂,主要解决现有技术中存在的环己烷直接氧化制己二酸反应中,自由基催化剂容易失活分解的问题。通过采用环己烷直接氧化制己二酸的自由基保护剂,包括柠檬酸和/或如下式所示的取代酚中的至少一种;其中,X和Y独立选自H或叔丁基,且X和Y不同时为H的技术方案,较好地解决了该问题,可用于环己烷直接氧化制己二酸的工业生产。

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20-10-1987 дата публикации

Method for preparing spirobiindane bisphenols

Номер: US4701566A
Принадлежит: General Electric Co

Spirobiindane bisphenols are prepared by contacting a mixture of a bisphenol or a 4-isopropenylphenol and a 1-(4-hydroxyphenyl)indanol with a metal halide Lewis acid or an alkanesulfonic acid. High purity spirobiindane bisphenols may be prepared by employing a purification sequence, which preferably includes a step of precipitation of the product with water from a methanol-methylene chloride solution.

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22-09-1992 дата публикации

Nitrogen-containing aromatic heterocyclic ligand-metal complexes and their use for the activation of hydrogen peroxide and dioxygen in the reaction of organic compounds

Номер: US5149880A
Принадлежит: TEXAS A&M UNIVERSITY SYSTEM

Nitrogen-containing aromatic heterocyclic ligand-metal complexes and their use for the activation of hydrogen peroxide and dioxgen are disclosed. Processes whereby activated hydrogen peroxide or dioxygen are used to transform various organic substrates are also disclosed. In particular, processes for the conversion of methylenic carbons to carbonyls, for the dioxygenation of aryl olefins, acetylenes and aryl-α-diols, for the oxidation of alcohols and aldehydes and for the removal of mercaptans from gaseous streams and for the removal of hydrogen sulfide and/or mercaptans from liquid streams are disclosed.

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18-10-2000 дата публикации

己二酸生产中从环己烷中除去乙酸的方法和装置

Номер: CN1270578A
Принадлежит: RPC Inc

本发明涉及一种在将环己烷直接氧化成己二酸的过程中,从环己烷中除去乙酸的方法和装置,特别是在循环催化剂以后,其中催化剂是通过引入附加的环己烷而沉淀的。乙酸的除去优选通过在一至三级萃取槽中使用相当少量的洗涤水来进行。由于更为有效,两级反应器是优选的。

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04-09-2018 дата публикации

Concerted processes for forming 1,2,4-trihydroxybenzene from hydroquinone

Номер: US10065977B2

Flow batteries incorporating an active material with one or more catecholate ligands can have a number of desirable operating features. Commercial syntheses of catechol produce significant quantities of hydroquinone as a byproduct, which presently has limited value in the battery industry and can represent a significant waste disposal issue at industrial production scales. Using a concerted, high-yield process, low-value hydroquinone can be transformed into high-value 1,2,4-trihydroxybenzene, which can be a desirable ligand for active materials of relevance in the flow battery industry. Methods for forming 1,2,4-trihydroxybenzene can include: oxidizing hydroquinone in a first reaction to form p-benzoquinone, converting the p-benzoquinone in a second reaction to form 1,2,4-triacetoxybenzene, deacetylating the 1,2,4-triacetoxybenzene in a third reaction to form 1,2,4-trihydroxybenzene, and isolating the 1,2,4-trihydroxybenzene after performing the first reaction, the second reaction and the third reaction consecutively.

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01-10-1998 дата публикации

PROCESS TO PRODUCE 2-METHYL-1,4-NAPHTOQUINONE.

Номер: ES2119283T3
Принадлежит: Kuraray Co Ltd

LA PRESENTE INVENCION PROPORCIONA UN PROCESO PARA PRODUCIR 2METIL-1,4-MAFTOQUINONA CARACTERIZADO POR LA REACCION ENTRE 2METILNAFTALENO Y PEROXIDO DE HIDROGENO Y/O UN PERACIDO ORGANICO EN UN SOLVENTE QUE INCLUYE UN ACIDO CARBOXILICO EN LA PRESENCIA ED UN COMPUESTO DE PALADIO Y ACIDO SULFURICO. THE PRESENT INVENTION PROVIDES A PROCESS TO PRODUCE 2METIL-1,4-MAFTOQUINONA CHARACTERIZED BY THE REACTION BETWEEN 2METILNAFTALENO AND HYDROGEN PEROXIDE AND / OR AN ORGANIC SOLUID THAT IS PRESENT IN AURICA, PRESIDENT OF AURICA, PRESIDENT OF AURO, AURO .

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05-07-2019 дата публикации

从氢醌形成1,2,4-三羟基苯的协同方法

Номер: CN109983123A
Принадлежит: Lockheed Martin Energy LLC

本发明公开了包含具有一个或多个儿茶酚配体的活性材料的液流电池可具有许多期望的工作特征。儿茶酚的商业合成产生大量的氢醌作为副产物,所述副产物目前在电池工业中的价值有限并且可造成工业生产规模上的重大废物处理问题。使用协同的高收率工艺,可以将低价值的氢醌转变为高价值的1,2,4‑三羟基苯,所述1,2,4‑三羟基苯可以是液流电池工业中相关的活性材料的理想配体。形成1,2,4‑三羟基苯的方法可包括:在第一反应中氧化氢醌以形成对苯醌,在第二反应中转化对苯醌以形成1,2,4‑三乙酰氧基苯,在第三反应中将1,2,4‑三乙酰氧基苯脱乙酰化以形成1,2,4‑三羟基苯,以及在接连进行第一反应、第二反应和第三反应后分离1,2,4‑三羟基苯。

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25-07-1991 дата публикации

Nitrogen-containing aromatic heterocyclic ligand-metal complexes and their use for the activation of hydrogen peroxide and dioxygen in the reaction of organic compounds

Номер: WO1991010634A1
Принадлежит: TEXAS A&M UNIVERSITY SYSTEM

Nitrogen-containing aromatic heterocyclic ligand-metal complexes and their use for the activation of hydrogen peroxide and dioxygen are disclosed. Processes whereby activated hydrogen peroxide or dioxygen are used to transform various organic substrates are also disclosed. In particular, processes for the conversion of methylenic carbons to carbonyls, for the dioxygenation of aryl olefins, acetylenes and aryl-$g(a)-diols, for the oxidation of alcohols and aldehydes and for the removal of mercaptans from gaseous streams and for the removal of hydrogen sulfide and/or mercaptans from liquid streams are disclosed.

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15-05-1995 дата публикации

테트라클로로-1, 4-벤조퀴논의 제조 방법

Номер: KR950011390A

본 발명은 사용되는 하이드로퀴논의 일부를 촉매량의 철(Ⅲ) 이온 및 음이온성 분산제를 함유하는 초기에 도입된 4- 내지 6-배 몰량(하이드로퀴논의 총 몰량을 기준으로 함)의 20 내지 37% 수성 염산에 도입하고, 20 내지 90℃의 온도에서 총 하이드로퀴논을 기준으로 1.5 내지 2.0배 몰량의 염소를 기체로서 상기 용액에 도입하고, 이어서 나머지량의 하이드로퀴논을 고체로서 또는 용해된 형태로 가하고, 1.5 내지 2.0배 몰량의 염소를 기체로서 도입하고, 물을 첨가하여 염산의 농도를 23 내지 25%로 유지시키고, 최종적으로 염소(1.7 내지 2.5배 몰량)를 기체로서 추가로 도입하고 염산 농도가 20 내지 22%가 되도록 물로 희석하면서 온도를 100 내지 107℃로 승온시킴을 포함하는, 하이드로퀴논상에서의 염소 및 진한 염산의 작용에 의해 고순도의 테트라클로로-1, 4-벤조퀴논을 제조하는 방법에 관한 것이다.

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19-03-1986 дата публикации

熱応答性バイオカプセル

Номер: JPS6154978A
Принадлежит: Mitsubishi Paper Mills Ltd

(57)【要約】本公報は電子出願前の出願データであるた め要約のデータは記録されません。

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20-08-2003 дата публикации

Method for oxidation of hydrocarbons

Номер: RU2210562C2

FIELD: organic chemistry, chemical technology. SUBSTANCE: invention relates to method for the direct oxidation of hydrocarbon taken among cycloalkanes where their cycle comprises from 5 to 12 carbon atoms up to carboxylic acid using oxygen or oxygen-containing gas in liquid phase in solvent taken among polar protonic and aprotonic solvents in the presence of catalyst dissolved in medium. Catalyst comprises at least one soluble cobalt compound and at least one soluble chrome compound taken in the molar ratio chrome to cobalt in catalyst from 0.001 to 1000 but preferably from 0.01 to 10. Method allows preparing the end product with high selectivity up to 67.3+ACU- being without using nitric acid that excludes treatment of nitrogen oxides. EFFECT: improved method of oxidation. 11 cl с99З0гсс ПЧ сэ РОССИЙСКОЕ АГЕНТСТВО ПО ПАТЕНТАМ И ТОВАРНЫМ ЗНАКАМ (19) (51) МПК? ВИ "” 2 210 562 ' 13) С2 С 07С 51/215, 55/14 12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ РОССИЙСКОЙ ФЕДЕРАЦИИ (21), (22) Заявка: 98106628/04, 09.04.1998 (24) Дата начала действия патента: 09.04.1998 (30) Приоритет: 10.04.1997 ЕК 9704637 (43) Дата публикации заявки: 21.01.2000 (46) Дата публикации: 20.08.2003 (56) Ссылки: АСАНО ЯСУСИ И ДР. Получение адипиновой кислоты. РЖХим, ВИНИТИ. - 1972, 13(1), реф. 13Н27. Ц$ 4658056 А, 14.04.1987. 5Ц 1659391 А\, 30.06.1991. $0 269138 А, 29.09.1977. 50 929213 А, 23.05.1982. СВ 1250192 А, 20.10.1971. СВ 415172 А, 23.08.1934. 5Ц 982319 АЛ, 10.11.1996. (98) Адрес для переписки: 129010, Москва, ул. Б. Спасская, 25, стр.3, ООО "Юридическая фирма Городисский и Партнеры", пат.пов. Н.Г.Лебедевой, рег. № 112 М., (71) Заявитель: РОДЬЯ ФИБЕР Э РЕЗЭН ЭНТЕРМЕДИАТ (ЕК) (72) Изобретатель: КОСТАНТИНИ Мишель (ЕК), ФАШ Эрик (ЕВ) (73) Патентообладатель: РОДЬЯ ФИБЕР Э РЕЗЭН ЭНТЕРМЕДИАТ (ЕК) (74) Патентный поверенный: Лебедева Наталья Георгиевна (54) СПОСОБ ОКИСЛЕНИЯ УГЛЕВОДОРОДОВ (57) Изобретение относится К усовершенствованному способу прямого окисления углеводорода, выбранного из циклоалканов, цикл ...

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12-08-1980 дата публикации

Image forming material comprising polyacids of Mo or W or their salts or complexes

Номер: US4217409A
Принадлежит: DAI NIPPON PRINTING CO LTD

There is provided an image-forming material of a laminar structure comprising: a substrate; an image-forming layer provided on at least one surface of the substrate and containing an image-forming agent selected from the group consisting of polyacids of molybdenum and tungsten and salts and complexes of these polyacids; and a transparent polymer film provided on the image-forming layer, at least one of the image-forming layer and the transparent polymer film containing a reducing agent. The image-forming material may be used in a one-stage image-forming process comprising irradiation thereof with image-wise light-rays including ultraviolet and visible and/or infrared rays or a two-stage image-forming process comprising irradiation thereof with image-wise ultra-violet rays and then with visible and/or infrared rays.

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15-12-1993 дата публикации

Patent JPH0587105B2

Номер: JPH0587105B2
Автор: Yutaka Masuda

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10-08-2016 дата публикации

一种生产甲酚的方法

Номер: CN103896740B
Автор: 刘中民, 徐云鹏, 王坤院

本发明提供了一种生产甲酚的方法,在反应温度250‑450℃、进料重量空速0.3‑5h ‑1 、常压反应条件下,将包含醚、酚和甲醇的原料经预热后与水蒸气混合连续通过多段固体催化剂床层,进行气相反应生成甲酚,其中所述固体催化剂选自氧化铝、高岭土和分子筛催化剂中一种或多种,所述酚选自苯酚、二甲酚和它们的混合物;所述醚选自苯甲醚、二甲醚、甲基苯甲醚或它们任意两种或多种的混合物。甲酚单程收率0.2g甲酚/g催化剂.时,对甲酚的对位选择性可达45%。催化剂稳定性好,生产过程中无设备腐蚀,是一种环境友好的催化剂,具有良好的工业应用前景。

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01-05-2000 дата публикации

Method for 1,4-naphthoquinones and anthraquinones using the [2+4] deils-alder reaction

Номер: KR100255547B1
Принадлежит: 금호석유화학주식회사, 박찬구

PURPOSE: Provided is a method for synthesizing 1,4-naphthoquinones and anthraquinones using£2+4|Diels-Alder reaction in high yield where resultant compounds from the£2+4|Diels-Alder reaction are continuously dehydrogenated in the same reactor as the£2+4|Diels-Alder reaction is carried out. Also, nitro compounds acting as solvent and oxidant are used in the£2+4|Diels-Alder reaction so that amine compounds can be obtained. CONSTITUTION: The preparation method of 1,4-naphthoquinones and anthraquinones comprises the process of reacting quinones selected from 1,4-benzoquinone, 2-methylbenzoquinone, 1,4-naphthoquinone with 1,3-butadienes selected from 1,3-butadiene, isoprene, 2,3-dimethyl-butadiene by using£2+4|Diels-Alder reaction where nitro compounds selected from nitrobenzene, p-nitrotoluene, and p-nitrophenol are used as both solvent and oxidant; continuously dehydrogenating resultant compounds. In the method, the temperature of the£2+4|Diels-Alder reaction is 140 to 210deg.C.

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25-01-1986 дата публикации

Preparation of 2,3,5-trimethylbenzoquinone

Номер: JPS6117532A
Принадлежит: Mitsubishi Gas Chemical Co Inc

(57)【要約】本公報は電子出願前の出願データであるた め要約のデータは記録されません。

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28-04-2017 дата публикации

Method of producing 2,6-dimethylbenzoquinone

Номер: EA201692246A1
Принадлежит: ДСМ АйПи АССЕТС Б.В.

Настоящее изобретение относится к усовершенствованному способу получения 2,6-диметилбензохинона (2,6-DMQ). The present invention relates to an improved method for producing 2,6-dimethylbenzoquinone (2,6-DMQ).

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25-11-1999 дата публикации

Controlled oxidation of hydrocarbons to intermediate oxidation products

Номер: WO1999059953A1
Принадлежит: Rpc, Inc.

This invention relates to methods of controlling the oxidation of hydrocarbons to respective intermediate oxidation products, e.g., dibasic acids, by adjusting the bulk temperature of the liquid mixture under oxidation by a cooling element, the temperature of which is maintained above a temperature at which solids deposit on the element or a second liquid phase is formed on the element, and/or by maintaining the oxygen concentration in the condenser off-gases to a level preferably lower than 90 % by volume of the flammable oxygen concentration, and/or by feeding oxygen and inert gas (preferably nitrogen) in the reaction zone, the inert gas and the oxygen having a ratio of inert gas to oxygen in the range of preferably 1:5 to 1:200. This invention is particularly applicable in the case of direct oxidation of cyclohexane to adipic acid.

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23-01-2001 дата публикации

Devices for removing acetic acid from cyclohexane in the production of adipic acid

Номер: US6177053B1
Принадлежит: RPC Inc

This invention relates to methods and devices for removing acetic acid from cyclohexane in the direct oxidation of cyclohexane to adipic acid, especially after recycling catalyst which is precipitated by introduction of additional cyclohexane. The removal of acetic acid is preferably conducted by use of rather small amounts of wash-water in one to three stage extractors. A two stage reactor is preferable as being more efficient.

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06-02-2001 дата публикации

Devices for controlling the reaction rate of a hydrocarbon to an intermediate oxidation product by pressure drop adjustments

Номер: US6183698B1
Принадлежит: RPC Inc

Devices for controlling the reaction rate of a hydrocarbon to an acid or other intermediate oxidation product by pressure drop rate adjustments. The devices incorporate a reaction chamber, different means for monitoring miscellaneous parameters, means for feeding ingredients including gases, means for exiting products and gases, means for stopping the feeding and exiting of gases at predetermined time intervals, means for measuring the pressure drop rate during the period that the feeding and exiting of gases takes effect, and a controller, the function of which is to conduct adjustments in one or more of temperature, feeding rates of hydrocarbon, solvent, catalyst, promoter, and the like until the pressure drop rate and the reaction rate fall within desirable predetermined limits.

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20-12-2001 дата публикации

Devices for controlling the reaction rate and/or reactivity of hydrocarbon to an intermediate oxidation product by adjusting the oxidant consumption rate

Номер: US20010053864A1
Принадлежит: Individual

Methods and devices for controlling the reaction rate and/or reactivity of a hydrocarbon to an intermediate oxidation product, such as an acid, within predetermined limits, are disclosed. Control of the reaction rate and/or reactivity within predetermined limits is achieved by monitoring and controlling the oxidant consumption rate. According to the present invention, examples of ways to determine the oxidant consumption rate include, but are not limited to, monitoring the flow rates of incoming and outgoing oxidant, monitoring pressure differentials after temporarily ceasing entry and exit of gases, and monitoring the flow rates of incoming and outgoing gases, and monitoring the rates of incoming and outgoing hydrocarbon. The methods and devices of the present invention are particularly advantageous in the case that the hydrocarbon is cyclohexane, the intermediate oxidation product is adipic acid, the solvent is acetic acid, the catalyst is cobalt (II) acetate tetrahydrate, and the initiator or promoter is cyclohexane, or acetaldehyde, or a mixture of thereof.

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19-10-1955 дата публикации

A method for the oxidation of cycloalkanes

Номер: GB738808A
Автор:

A method of oxidizing cycloalkanes comprises the steps of subjecting a cycloalkane containing at least four cyclic carbon atoms to oxidation by means of a free-oxygen-containing gas at a temperature of from 100 DEG to 200 DEG C. and at a pressure at least sufficient to maintain the cycloalkane in the liquid phase, separating the resultant reaction mixture into an upper liquid hydrocarbon-rich phase and a lower phase rich in oxy-compounds containing water and some dissolved hydrocarbons, distilling the liquid oxy-compound-rich phase so as to remove hydrocarbons and water therefrom, withdrawing the residual material containing the oxy compounds from which the water and hydrocarbons have been removed from the distillation step; and further oxidizing this residual material by <PICT:0738808/IV (b)/1> means of a free-oxygen-containing gas at a temperature of from 100 DEG to 170 DEG C. and at a pressure at least sufficient to maintain the residual material in the liquid phase. Cycloalkanes mentioned are cyclohexane, cyclopentane, cyclobutane or homologues such as the methyl-, dimethyl-, ethyl-substituted cyclic hydrocarbons or their homologues with the production of the corresponding dibasic acids such as adipic, glutaric or succinic acids or their homologues. The products also include ketones and alcohols, e.g. from cyclohexane adipic acid, cyclohexanol and cyclohexanone are obtained. Catalysts which may be used include polyvalent metals of atomic weights between 50 and 200 which may be used in the finely divided state or as organic or inorganic salts or oxides. Specific metals include cerium, cobalt, copper, manganese and uranium. Specific catalysts mentioned include vanadium, cerium and cobalt chlorides, manganese naphthenate, manganese acetate alone or together with barium or cobalt permanganate, sodium cobaltinitrite or mixtures of two or more of such compounds. Promoters which may also be present include salts of alkali- and alkaline-earth metals, e.g. barium, ...

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19-10-1976 дата публикации

Cyclohexane oxidation in the presence of binary catalysts

Номер: US3987100A
Принадлежит: EI Du Pont de Nemours and Co

The process of oxidizing cyclohexane to produce cyclohexanone and cyclohexanol in the weight ratio of 0.5 to 1.5 of cyclohexanone to cyclohexanol, said process comprising contacting a stream of liquid cyclohexane with oxygen in each of at least three successive oxidation stages by introducing into each stage a mixture of gases comprising molecular oxygen and inert gas, said oxygen being introduced in amounts that may range from an amount that will substantially all react with the cyclohexane under the particular conditions involved to an amount in excess of the amount required to react with the cyclohexane, said excess being such that the overall oxygen consumed in the oxidation zone is not more than 95 mole percent of the amount fed under the particular conditions involved, in the presence of a binary catalyst system comprising 0.02 to 0.9 ppm chromium and 0.1 to 5 ppm cobalt at a temperature of from 130° to 200° C. and a pressure of from 60 to 350 psig, reacting any cyclohexylhydroperoxide that may be formed in the presence of said binary catalyst system and recovering a product of cyclohexanone and cyclohexanol in the above ratio.

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22-06-1993 дата публикации

One step air oxidation of cyclohexane to produce adipic acid

Номер: US5221800A
Принадлежит: BP Corp North America Inc

A process for the manufacture of adipic acid is disclosed. In this process, cyclohexane is oxidized in an aliphatic monobasic acid solvent in the presence of a soluble cobalt salt wherein water is continuously or intermittently added to the reaction system after the initiation of oxidation of cyclohexane as indicated by a suitable means of detection, and wherein the reaction is conducted at a temperature of about 50° C. to about 150° C. at an oxygen partial pressure of about 50 to about 420 pounds per square inch absolute.

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14-06-1994 дата публикации

Process for the preparation of adipic acid and other aliphatic dibasic acids

Номер: US5321157A
Автор: John Kollar
Принадлежит: Redox Technologies Inc

The present invention relates to a process for the preparation of C 5 -C 8 aliphatic dibasic acids through oxidation of corresponding saturated cycloaliphatic hydrocarbons by (1) reacting, at a cycloaliphatic hydrocarbon conversion level of between about 7% and about 30%, (a) at least one saturated cycloaliphatic hydrocarbon having from 5 to 8 ring carbon atoms in the liquid phase and (b) an excess of oxygen gas or an oxygen-containing gas mixture in the presence of (c) less than 1.5 moles of a solvent per mole of cycloaliphatic hydrocarbon (a), wherein said solvent comprises an organic acid containing only primary and/or secondary hydrogen atoms and (d) at least about 0.002 mole per 1000 grams of reaction mixture of a polyvalent heavy metal catalyst; and (2) isolating the C 5 -C 8 aliphatic dibasic acid.

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31-10-1995 дата публикации

Recycling process for the production of adipic acid and other aliphatic dibasic acids

Номер: US5463119A
Автор: John Kollar
Принадлежит: Redox Technologies Inc

The invention relates to a process for the oxidative preparation of C 5 -C 8 aliphatic dibasic acids by (1) reacting (a) at least one saturated cycloaliphatic hydrocarbon having from 5 to 8 ring carbon atoms in the liquid phase and (b) an excess of an oxygen-containing gas in the presence of (c) a solvent comprising an organic acid containing only primary and/or secondary hydrogen atoms and (d) at least about 0.002 mole per 1000 grams of reaction mixture of a polyvalent heavy metal catalyst; (2) removing the aliphatic dibasic acid; and (3) recycling intermediates, post-oxidation components, and derivatives thereof remaining after removal of the aliphatic dibasic acid into the oxidation reaction.

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08-02-1966 дата публикации

Adipic acid production by the two step oxidation of cyclohexane with oxygen

Номер: US3234271A
Принадлежит: Halcon International Inc

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02-01-1968 дата публикации

Process for oxidizing cyclohexane to adipic acid

Номер: US3361806A
Автор: Rex E Lidov
Принадлежит: Halcon International Inc

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02-06-1970 дата публикации

Process for oxidation of cyclohexane

Номер: US3515751A
Принадлежит: Firestone Tire and Rubber Co

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08-08-2001 дата публикации

Controlled oxidation of hydrocarbons to intermediate oxidation products

Номер: CN1307555A
Принадлежит: RPC Inc

本发明涉及通过借助冷却元件调整进行氧化的液体混合物的整体温度来实现烃控制氧化为对应中间氧化产物如己二酸的方法,所述冷却元件的温度保持在高于固体沉积在所述元件上或在所述元件上形成第二液体的温度,和/或通过将冷凝器排出气中的氧浓度保持在优选低于易燃氧浓度90vol%来实现所述方法,和/或通过在反应区中加入氧和惰性气体(优选氮)实现所述方法,所述惰性气体与氧的比值范围优选为1∶5至1∶200。本发明特别适用于环己烷直接氧化为己二酸的情况。

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23-11-2001 дата публикации

Method of Separating Catalysis in Solution from A Reaction Produced by Oxidation of Cyclohexane to Adipic Acid

Номер: KR20010103554A

본 발명은 반응영역 바깥에서 반응혼합물에서 촉매제를 추출하여 1염기산 용매의 존재하에 시클로헥산의 아디프산으로의 산화를 제어하는 방법에 관한 것이다. 대체로 모든 반응하지 않은 시클로헥산, 대부분의 아디프산 그리고 모든 1염기산 용매를 가급적이면 반응산물에서 분리한다. 실질적으로 모든 1염기산 용매가 분리되는 경우, 1염기산을 분리하는 동안 프로톤성 용매는 고체침전을 방지하기 위해 가급적이면 정제에 의해 프로톤성 용매는 간헐적 또는 연속적으로 반응혼합물에 첨가될 것이다. 그 후, 단일 액상을 유지하기에 적절한 양의 프로톤성 용매(새로운 화합물 용매를 구성하는 쌍극성 비프로톤성 용매 및 프로톤성 용매 총량)의 존재 하에 쌍극성 비프로톤성 용매를 첨가한 후, 프로톤성 용매 내의 모든 촉매제를 실질적으로 추출하는 한 단계를 거친다. 촉매제 추출물은 가급적이면 시크롤헥산이 아디프산으로 산화되는 곳인 반응영역으로 리사이클된다. 이와 같이, 바람직하게는 시클로헥산과 물의 조합인 새로운 화합물 용매는 가급적이면 대부분의 아디프산을 분리 완전히 추출된다. 촉매제 침전은 일어나지 않고, 고형질을 다루는 데 대한 모든 불편사항 및 지출이 방지된다.

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18-04-2001 дата публикации

Methods of separating catalyst in solution from a reaction mixture produced by oxidation of cyclohexane to adipic acid

Номер: EP1091921A1
Принадлежит: RPC Inc

This invention relates to methods of controlling the oxidation of cyclohexane to adipic acid in the presence of a monobasic acid solvent, by separating the catalyst from the reaction mixture, outside the reaction zone. Substantially all the unreacted cyclohexane, the majority of adipic acid, and substantially all the monobasic acid solvent are preferably removed. A protic solvent, may be added intermittently or continuously in the reaction mixture during the removal of the monobasic acid solvent, preferably by distillation, for preventing solids precipitation. A dipolar aprotic solvent is then added in the presence of an adequate amount of the protic solvent to maintain a single liquid phase, followed by a step of formation of two liquid phases, a solids-free protic liquid phase containing substantially all the catalyst, and a solids-free aprotic liquid phase containing at least the majority of ingredients of the reaction mixture. The formation of the two phases is performed by a process selected from a group consisting of lowering the first temperature to a second temperature, adding additional protic solvent, adding an apolar aprotic solvent, and a combination thereof.

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02-07-2002 дата публикации

Method for separating catalyst in solution from reaction mixture formed by oxidation of cyclohexane to adipic acid

Номер: JP2002519400A

(57)【要約】 本発明は、反応混合物から触媒を、反応ゾーンの外側に分離することによって、一塩基酸溶媒の存在下における、シクロヘキサンからアジピン酸への酸化を制御する方法に関する。好ましくは、実質的に全ての未反応のシクロヘキサン、大部分のアジピン酸、および実質的に全ての一塩基酸が除去される。一塩基酸溶媒が好ましくは蒸留によって除去される間に、プロトン性溶媒が、固体の沈殿を避けるために、反応混合物に断続的または連続的に添加され得る。次いで、両性の非プロトン性溶媒が、単一液相を保持するのに適量のプロトン性溶媒の存在下で添加され、次いで、2つの液相(実質的に全ての触媒を含有する、固体を含有しないプロトン性液相、および反応混合物の少なくとも大部分の成分を含有する、固体を含有しない非プロトン性液相)が形成する。この2つの相の形成は、第1温度から第2温度に下げる工程、追加のプロトン性溶媒を添加する工程、無極性の非プロトン性溶媒を添加する工程、およびそれらの組み合わせからなる群から選択されるプロセスによって行われる。

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22-08-2001 дата публикации

Methods of extracting catalyst from reaction mixture in oxidation of cyclohexane to adipic acid

Номер: CN1309627A
Принадлежит: RPC Inc

本发明涉及通过在反应区之外从反应混合物中萃取催化剂控制在一元酸溶剂存在下环己烷至己二酸的氧化的方法。从反应产物中除去基本上所有未反应的环己烷、大部分己二酸、和优选基本上所有一元酸溶剂。在除去基本上所有一元酸溶剂的情况下,在除去所述一元酸溶剂(优选通过蒸馏)期间间歇或连续地向反应混合物中加质子传递溶剂以防止固体沉淀。然后在足以保持单液相的足量质子传递溶剂存在下加入偶极非质子传递溶剂(偶极非质子传递溶剂和所述质子传递溶剂之总体构成新的组合溶剂),接着将基本上所有催化剂萃取在质子传递溶剂中。所述催化剂萃取液优选循环至反应区,在所述反应区使环己烷氧化成己二酸。这样,所述新组合溶剂(优选环己酮与水组合)使反应产物溶解,优选在除去大部分己二酸之后,然后所述催化剂基本上全部萃取至水中。不发生催化剂沉淀,防止了处理固体的所有缺点和成本。

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13-01-2000 дата публикации

Methods of separating catalyst in solution from a reaction mixture produced by oxidation of cyclohexane to adipic acid

Номер: CA2337792A1
Принадлежит: Individual

This invention relates to methods of controlling the oxidation of cyclohexane to adipic acid in the presence of a monobasic acid solvent, by separating the catalyst from the reaction mixture, outside the reaction zone. Substantially all the unreacted cyclohexane, the majority of adipic acid, and substantially all the monobasic acid solvent are preferably removed. A protic solvent, may be added intermittently or continuously in the reaction mixture during the removal of the monobasic acid solvent, preferably by distillation, for preventing solids precipitation. A dipolar aprotic solvent is then added in the presence of an adequate amount of the protic solvent to maintain a single liquid phase, followed by a step of formation of two liquid phases, a solids-free protic liquid phase containing substantially all the catalyst, and a solids-free aprotic liquid phase containing at least the majority of ingredients of the reaction mixture. The formation of the two phases is performed by a process selected from a group consisting of lowering the first temperature to a second temperature, adding additional protic solvent, adding an apolar aprotic solvent, and a combination thereof.

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13-01-2000 дата публикации

Methods of separating catalyst in solution from a reaction mixture produced by oxidation of cyclohexane to adipic acid

Номер: WO2000001655A1
Принадлежит: Rpc Inc.

This invention relates to methods of controlling the oxidation of cyclohexane to adipic acid in the presence of a monobasic acid solvent, by separating the catalyst from the reaction mixture, outside the reaction zone. Substantially all the unreacted cyclohexane, the majority of adipic acid, and substantially all the monobasic acid solvent are preferably removed. A protic solvent, may be added intermittently or continuously in the reaction mixture during the removal of the monobasic acid solvent, preferably by distillation, for preventing solids precipitation. A dipolar aprotic solvent is then added in the presence of an adequate amount of the protic solvent to maintain a single liquid phase, followed by a step of formation of two liquid phases, a solids-free protic liquid phase containing substantially all the catalyst, and a solids-free aprotic liquid phase containing at least the majority of ingredients of the reaction mixture. The formation of the two phases is performed by a process selected from a group consisting of lowering the first temperature to a second temperature, adding additional protic solvent, adding an apolar aprotic solvent, and a combination thereof.

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03-01-2006 дата публикации

Methods and apparatus for removing catalyst from oxidation reactor effluent

Номер: US6982234B2
Принадлежит: GTC Technology Inc

Methods and apparatus for removing a catalyst from a reaction mixture formed by reacting a hydrocarbon or an oxygenated hydrocarbon with an oxidant in the presence of the catalyst in a reactor, in which the reaction mixture contains one or more dibasic acids. The catalyst is removed by adding water and/or cooling the reaction mixture to cause phase separation, recycling the polar phase to the reactor, and transferring the less-polar phase to an ion exchange unit to remove catalyst contained therein.

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25-06-1968 дата публикации

Process for the preparation of adipic acid

Номер: US3390174A
Принадлежит: Gulf Research and Development Co

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14-03-1972 дата публикации

Process for the preparation of adipic acid

Номер: US3649685A
Принадлежит: Teijin Ltd

A PROCESS FOR THE PREPARATION OF ADIPIC ACID WHICH COMPRISES OXIDIZING CYCLOHEXANE WITH MOLECULAR OXYGEN IN ACETC ACID SOLVENT AT TEMPERTURES RANGING FROM 85* TO 120*C., IN THE CONCURRENT PRSENCE OF AN ORGANIC CARBOXYLATE OF COBALT SUCH AS COBALT ACETATE AND A BROMINE COMPOUND SUCH AS AN ALKALI METAL BROMIDE AND AN ALKALINE EARTH METAL BROMIDE AT SUCH A RATIO THAT THE ATOMIC RATIO OF BR TO CO RANGES FRM 1X10-4 TO 1:1 AND RECOVERING THE FORMED ADIPIC ACID. THUS, ADIPIC ACID IS FORMED WITH HIGH CONVERSION AND WITH AN EXTREMELY SHORT INDUCTION PERIOD, AND THE CARBOXYLATE OF COBALT AND BROMINE COMPOUND OF THE CATALYST SYSTEM CAN BE RECOVERED.

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28-06-1977 дата публикации

Process for converting cyclohexane to adipic acid

Номер: US4032569A
Принадлежит: Gulf Research and Development Co

A process for converting cyclohexane to adipic acid which involves oxidizing cyclohexane with molecular oxygen in the presence of critical amounts of cobaltic ions in an aliphatic monobasic acid while maintaining critical temperature, pressure and contact time in the reaction zone.

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19-06-1979 дата публикации

Process for converting cyclopentane to glutaric acid

Номер: US4158739A
Принадлежит: Gulf Research and Development Co

A process for converting cyclopentane to glutaric acid which involves oxidizing cyclopentane with molecular oxygen in the presence of critical amounts of cobaltic ions in an aliphatic monobasic acid while maintaining critical temperature, pressure and contact time in the reaction zone.

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