Process for Preparing Caprolactam and Polyamides Therefrom

Provided herein are processes for preparing caprolactam from a starting material such as one or more of the cis,cis-, cis,trans- and trans,trans-double-bond isomers of muconamide, muconic acid ester, or muconic acid. The starting material, intermediates, and caprolactam prepared therefrom can contain carbon atoms derived from biomass containing detectable C content determined according to ASTM D6866 and optionally containing a C content up to 0.0000000001% (one part per trillion). Caprolactam so prepared can be used to make various polyamides. 2. The process of claim 1 , wherein the reacting step comprises reactions via Route 1:{'sub': 2', '3, 'converting Q,Q-MA to caprolactam 1 in an aprotic polar solvent, using Hand NHgases at a total initial pressure from about 250 to about 2050 psi, at a temperature from about 200 to about 300° C., and in the presence of at least one catalyst.'}3. The process of claim 2 , wherein the aprotic polar solvent is 1 claim 2 ,4-dioxane claim 2 , diglyme or DMSO.4. The process of claim 2 , wherein the aprotic polar solvent is mixed with water or an alcohol.5. The process of claim 4 , wherein the alcohol is MeOH.6. The process of claim 2 , wherein the at least one catalyst comprises one or more of Pd claim 2 , Pt claim 2 , Rh and Ru.7. The process of claim 6 , wherein the at least one catalyst comprises Ru and Pt or Ru and Pd.8. The process of claim 2 , wherein the at least one catalyst is present at from about 0.3 to about 1 mol %.9. The process of claim 2 , wherein the converting step takes about 0.5 to about 3 hours.10. The process of claim 1 , wherein the reacting step comprises reactions via Route 2:{'sup': α', 'β, '(1) converting one or both of the cis,cis-MA and cis,trans-MA to one or both of Δ-muconolactone and Δ-muconolactone; and'}{'sup': α', 'β, 'sub': 2', '3, '(2) reacting one or both of Δ-muconolactone and Δ-muconolactone to form caprolactam 1, using Hand NHgases, and in the presence of at least one catalyst.'}11. The ...

PROCESSES FOR PRODUCING CAPROLACTAM AND DERIVATIVES THEREOF FROM FERMENTATION BROTHS CONTAINING DIAMMONIUM ADIPATE, MONOAMMONIUM ADIPATE AND/OR ADIPIC ACID

Processes for making caprolactam (CL) from monoammonium adipate (MAA) and/or adipic aicd (AA) obtained from a clarified diammonium adipate-containing (DAA-containing) fermentation broth or MAA-containing fermentation broth and converting the MAA or AA to the CL with hydrogen in the presence of a catalyst at selected temperatures and pressures. 1. A process for producing CL from a clarified DAA-containing fermentation broth , comprising:(a) distilling the broth to firm an overhead that comprises water and ammonia, and a liquid bottoms that comprises MAA, at least some DAA, and at least about 20 wt % water;{'sub': 'N', '(b) cooling andfor evarating the bottoms, and optionally adding an antisolvmt to the bottoms, to attain a temperature and composition sufficient to cause the bottoms to separate into a DAA-containing liquid portion and a MAA-containing, solid portion that is substantially free of DAA;'}(c) separating the solid portion from the liquid portion;(d) recovering the solid portion; and(e) contacting at least a portion of the solid portion with hydrogen, optionally in the presence of a solvent, in the presence of to hydrogenation catalyst and, optionally an ammonia source, at a temperature of about 25° C. to about 500° C. and a pressure of about 0.5 to about 40 MPa to produce the CL.2. A process for producing CI from a DAA-comairring fermentation broth , comprising:(a) distilling the broth to form a first overhead that includes water and ammonia, and a first liquid bottoms that includes MAA, at least some DAA, and at least about 20 wt % water;(b) cooling andlor evaporating the bottoms, and optionally adding an antisolvent to the bottoms, to attain a temperature and composition sufficient to cause the bottoms to separate into a DAA-containing liquid portion and a MAA-containing solid portion that is substantially free of DAA;(c) separating the solid portion from the liquid portion;(d) recovering the solid portion;(e) dissolvine the solid portion in Water to ...

PROCESSES FOR THE PRODUCTION OF HYDROGENATED PRODUCTS AND DERIVATIVES THEREOF

Processes for making hydrogenated products including caprolactame (CL) caprolactone (CLO) or 1,6-hexanediol (HDO) and derivative thereof from monoammonium adipate (MAA) and/or adipic acid (AA) obtained from a clarified diammonium adipate-containing (DAA-containing) fermentation broth or monoammonium adipate-containing (MAA-containing) fermentation broth. 1. A process for making a hydrogenated product from a clarified DAA-containing fermentation broth comprising;(a) distilling the broth to form an overhead that comprises water and ammonia, and a liquid bottoms that comprises MAA, at least some DAA, and at least about 20 wt % water;(b) cooling and/or evaporating the bottoms, and optionally adding an antisolvent to the bottoms, to attain a temperature and composition sufficient to cause the bottoms to separate into a DAA-containing liquid portion and a MAA-containing solid portion that is substantially free of DAA;(c) separating the solid portion from the liquid portion;(d) recovering the solid portion;(e) hydrogenating the solid portion in the presence of at least one hydrogenation catalyst to produce the hydrogenated product comprising at least one of CL, CLO or HDO; and(f) recovering the hydrogenated product.2. A process for making a hydrogenated product from a DAA-containing fermentation broth comprising:(a) distilling the broth to form a first overhead that includes water and ammonia, and a first liquid bottoms that includes MAA, at least some DAA, and at least about 20 wt % water;(b) cooling and/or evaporating the bottoms, and optionally adding an antisolvent to the bottoms, to attain a temperature and composition sufficient to cause the bottoms to separate into a DAA-containing liquid portion and a MAA-containing solid portion that is substantially free of DAA;(c) separating the solid portion from the liquid portion;(d) recovering the solid portion;(e) dissolving the solid portion in water to produce an aqueous MAA solution;(f) distilling the aqueous MAA ...

PRODUCTION METHOD OF INTERMEDIATE COMPOUND FOR SYNTHESIZING MEDICAMENT

The present invention relates to a novel method for preparing a compound of formula (2) as the intermediate, which can be effectively used for preparation of a compound of formula (1) exhibiting good inhibitory activity against dipeptidyl peptidase IV enzyme. 3. The method according to claim 1 , wherein Pis t-butyl group claim 1 , and Pis methyl or ethyl group.4. The method according to claim 1 , wherein GO is triflate claim 1 , mesylate claim 1 , tosylate claim 1 , besylate or nonaflate.5. The method according to claim 1 , wherein R3 and R4 are hydrogen claim 1 , and R5 and R6 are fluorine.6. The method according to claim 2 , wherein in step (a) C-Ctrialkylamine is used as the base.7. The method according to claim 2 , wherein in step (b) acetic acid is used as the acid.8. The method according to claim 2 , wherein in the case of the compound of formula (2a) wherein Pis Boc and Pis t-butyl claim 2 , the hydrolysis of said step (c) is conducted under the basic condition to selectively remove only Pamong the protecting groups Pand Pto provide the compound of formula (2).9. The method according to claim 8 , wherein aqueous sodium hydroxide solution is used as the base.11. The method according to claim 10 , wherein in step (a) the reduction is conducted using NaBH.12. The method according to claim 10 , wherein in step (b) the Gcompound is selected from the group consisting of trifluoromethane sulfonic acid anhydride (TfO) claim 10 , trifluoromethane sulfonyl chloride (TfCl) claim 10 , methanesulfonyl chloride (MsCl) claim 10 , toluenesulfonyl chloride (TsCl) claim 10 , bromobenzenesulfonyl chloride (BsCl) claim 10 , (CF(CF)SO)F and (CF(CF)SO)O.14. The method according to claim 13 , wherein Pis Boc claim 13 , Pis i-propyl group or t-butyl group claim 13 , and GO is triflate or nonaflate.17. The method according to claim 16 , wherein Pis Boc claim 16 , and Pis i-propyl or t-butyl.18. The method according to claim 16 , wherein in step (a) chloroformate or BocO is used as ...

ANTI-INFLAMMATORY AGENTS

Disclosed herein are methods of preventing or treating inflammatory diseases using 3-aminolactam compounds, each with aromatic “tail groups”. Compounds as defined by formulae (I) and (I′), and the medical uses of the compounds, are described herein. 3. (canceled)4. (canceled)6. A compound of{'claim-ref': {'@idref': 'CLM-00002', 'claim 2'}, ','}provided that the compound is not selected from the group consisting of: (S)-3-(4′-methoxybenzoylamino)-caprolactam, (S)-3-(4′-methylbenzoylamino)-caprolactam, (S)-3-(3′-trifluoromethylbenzoylamino)-caprolactam, (S)-3-(2′-carboxybenzoyl-amino)-caprolactam, and (S)-3-(3′,4′,5′-trimethoxybenzoylamino)-caprolactam.7. A pharmaceutical composition comprising claim 5 , as active ingredient claim 5 , a compound as defined in claim 5 , or a pharmaceutically acceptable salt thereof claim 5 , and at least one pharmaceutically acceptable excipient and/or carrier.8. The compound according to claim 1 , wherein n=2.9. The compound according to claim 1 , wherein n=3.10. The compound according to claim 1 , wherein X is haloalkyl.11. The compound according to claim 2 , wherein the compound is selected from the group consisting of:(S)-3-(4′-methylbenzoylamino)-caprolactam, and(S)-3-(3′,5′-dimethylbenzoylamino)-caprolactam,and pharmaceutically acceptable salts thereof.12. A compound according to claim 2 , selected from the group consisting of:(S)-3-fluoro-N-(2-oxopiperidin-3-yl)benzamide,(S)-2-fluoro-N-(2-oxopiperidin-3-yl)benzamide,(S)-4-fluoro-N-(2-oxopiperidin-3-yl)benzamide,(S)—N-(2-oxopiperidin-3-yl)-4-(trifluoromethyl)benzamide,(S)—N-(2-oxopiperidin-3-yl)-3-(trifluoromethyl)benzamide,(S)—N-(2-oxopiperidin-3-yl)-2-(trifluoromethyl)benzamide,(S)-2,3-difluoro-N-(2-oxopiperidin-3-yl)benzamide,(S)-2,4-difluoro-N-(2-oxopiperidin-3-yl)benzamide,(S)-2,5-difluoro-N-(2-oxopiperidin-3-yl)benzamide,(S)-2,6-difluoro-N-(2-oxopiperidin-3-yl)benzamide,(S)-3,4-difluoro-N-(2-oxopiperidin-3-yl)benzamide,(S)-3,5-difluoro-N-(2-oxopiperidin-3-yl)benzamide,(S)-3 ...

ANTI-INFLAMMATORY AGENTS

Disclosed herein are methods of preventing or treating inflammatory diseases using sulfonamide analogs of 3-aminolactam compounds, each with aromatic “tail groups”. Compounds as defined by formulae (I) and (I′), and the medical uses of the compounds, are described herein. 3. (canceled)4. (canceled)5. A compound according to claim 1 , with the proviso that:{'sub': 2', '6', '1', '7', '1', '7, 'when n =3, then at least one of C-Con the phenyl ring is substituted with a group other than halogen, C-Calkyl, or C-Chaloalkyl; and'}when n =1, 2 or 3, then{'sub': 2', '6, 'Cor Con the phenyl ring are other than hydrogen or fluorine, or'}{'sub': 3', '1', '6, 'Con the phenyl ring is other than hydrogen, halogen, C-Calkyl,'}{'sub': 1', '6', '1', '6, 'C-Calkoxy, or C-Chaloalkyl, or'}{'sub': 4', '1', '6', '1', '6', '1', '6, 'Con the phenyl ring is other than hydrogen, halogen, C-Calkyl, C-Calkoxy, C-Chaloalkyl, amino, aminoalkyl or aminodialkyl, or'}{'sub': '5', 'Con the phenyl ring is other than hydrogen or halogen;'}provided that the compound is neither of:3-(2′-carboxybenzenesulfonylamino)-tetrahydropyridin-2-one, and (R)-3-(4′-methylbenzenesulfonylamino)-caprolactam.6. A compound of claim 2 , with the proviso that:{'sub': 2', '6', '1', '7', '1', '7, 'when n=3, then at least one of C-Con the phenyl ring is substituted with a group other than halogen, C-Calkyl, or C-Chaloalkyl; and'}when n =1, 2 or 3, then{'sub': 2', '6, 'Cor Con the phenyl ring are other than hydrogen or fluorine, or'}{'sub': 3', '1', '6', '1', '6', '1', '6, 'Con the phenyl ring is other than hydrogen, halogen, C-Calkyl, C-Calkoxy, or C-Chaloalkyl, or'}{'sub': 4', '1', '6', '1', '6', '1', '6, 'Con the phenyl ring is other than hydrogen, halogen, C-Calkyl, C-Calkoxy, C-Chaloalkyl, amino, aminoalkyl or aminodialkyl, or'}{'sub': '5', 'Con the phenyl ring is other than hydrogen or halogen;'}provided that the compound is not one of the group consisting of:(S)-3-(4′-methylbenzenesulfonylamino)-tetrahydropyridin-2-one ...

HIGH TEMPERATURE LACTAM NEUTRALISATION

The invention relates to a method for preparing a lactam in a continuous process, comprising forming the lactam and ammonium sulphate by contacting a lactam sulphate contained in an acidic liquid with ammonia, during which forming of lactam heat of reaction is generated, which heat is partially or fully recovered, wherein ammonia is brought into contact with the acidic liquid as part of a liquid aqueous ammonia solution, and wherein the contacting takes place at a temperature of at least 120° C., and wherein the average residence time at a temperature of at least 120° C. is at most 15 minutes, and wherein the ammonium sulphate remains dissolved in a liquid phase during said residence time. 1. Method for preparing a lactam in a continuous process , comprising forming the lactam and ammonium sulphate by contacting a lactam sulphate contained in an acidic liquid with ammonia , during which forming of lactam heat of reaction is generated , which heat is partially or fully recovered , wherein ammonia is brought into contact with the acidic liquid as part of a liquid aqueous ammonia solution , wherein the contacting takes place at a temperature of at least 120° C. , and wherein the average residence time at a temperature of at least 120° C. is at most 15 minutes , and wherein the ammonium sulphate remains dissolved in a liquid phase during said residence time.2. Method according to claim 1 , wherein the heat is partially or fully used for steam generation claim 1 , preferably steam having a super-atmospheric pressure.3. Method according to claim 2 , wherein the heat is recovered by transferring the heat to a water stream via a heat exchanger claim 2 , which water stream is converted into a steam stream.4. Method according to claim 2 , wherein heat is transferred from product stream comprising lactam and ammonium sulphate claim 2 , and the product stream is thereafter subjected to (further) cooling to a temperature below 120° C. claim 2 , preferably below 100° C. claim 2 , ...

METHOD FOR MAKING ALPHA-AMINO-EPSILON-CAPROLACTAM USING MIXED SUPER CRITICAL FLUIDS

The present invention can involve a method of synthesizing α-amino-ε-caprolactam. The method can comprise heating a salt of L-lysine in a solvent comprising an alcohol under Super Critical Fluid conditions. The methods can comprise heating a salt of L-lysine in a solvent comprising an alcohol and deaminating the reaction product. In various embodiments, the invention can include methods of converting biomass into nylon 6. The methods can comprise heating L-lysine in a solvent comprising an alcohol to produce α-amino-ε-caprolactam, deaminating to produce ε-caprolactam and polymerizing into nylon 6, wherein the L-lysine is derived from biomass. In other embodiments, the present invention can include methods of making nylon 6. The methods can comprise synthesizing ε-caprolactam and then polymerizing, wherein the ε-caprolactam is derived from L-lysine. 1. A process for synthesizing a α-amino -ε-caprolactam , the process comprising:heating a salt of lysine in a solvent comprising: an alcohol, a water or an alcohol and a water, without the presence of a catalyst, at a temperature of about 235° C. to about 320° C., to produce the α-amino-ε-caprolactam.2. The process of according to claim 1 , further comprising:(a) purifying the α-amino-ε-caprolactam; or(b) crystallizing the α-amino-ε-caprolactam.3. (canceled)4. The process of claim 1 , wherein the lysine is L-lysine.5. The process of claim 1 , wherein the alcohol has from 2 to 6 carbons.6. The process of claim 1 , wherein the alcohol comprises a diol claim 1 , a triol claim 1 , a glycol claim 1 , or a combination thereof.78and . (canceled)9. The process of claim 1 , wherein the alcohol is selected from the group consisting of an ethanol claim 1 , a 1-propanol claim 1 , a 1-butanol claim 1 , a 1-pentanol claim 1 , a 1-hexanol claim 1 , a 1 claim 1 ,2-propanediol claim 1 , and mixtures thereof.10. The process of claim 1 , wherein the alcohol comprises a methanol claim 1 , an ethanol claim 1 , a butanol or a 1 claim 1 ,2- ...

CAPROLACTAM RECOVERY WITH MEMBRANE TREATMENT

The invention relates to a process for treating an aqueous solution containing ε-caprolactam, ammonium sulphate and one or more other impurities, comprising one or more organic impurities from a caprolactam production process and optionally other salts than ammonium sulphate, by means of a membrane process, thereby obtaining a retentate and a permeate, in which process the membrane used is selected from the group of polyether sulphone membranes, sulphonated polyether sulphone membranes, polyester membranes, polysulphone membranes, aromatic polyamide membranes, polyvinyl alcohol membranes, polypiperazine membranes, cellulose acetate membranes, titanium oxide membranes, zirconium oxide membranes and aluminium oxide membranes, having a molecular weight cut off in the range of 100-1000 g/mol; and wherein more than 60 wt. % of the caprolactam in the aqueous solution is passed through a membrane to the permeate side, to obtain a purified caprolactam containing permeate stream, and wherein at least 50 wt. % of the organic impurities are retained in the retentate solution.

PRODUCTION OF CAPROLACTAM FROM ADIPIC ACID

Processes are disclosed for the conversion of adipic acid to caprolactam employing a chemocatalytic reaction in which an adipic acid substrate is reacted with ammonia and hydrogen, in the presence of particular heterogeneous catalysts and employing unique solvents. The present invention also enables the conversion of other adipic acid substrates, such as mono-esters of adipic acid, di-esters of adipic acid, mono-amides of adipic acid, di-amides of adipic acid, and salts thereof to caprolactam. Solvents useful in the process that do not react with ammonia are also disclosed. Catalyst supports are disclosed which catalyze the reaction of the substrate with ammonia in the absence of added metal. Metals on the catalyst supports comprise ruthenium (Ru), rhodium (Rh), palladium (Pd), osmium (Os), iridium (Ir), and/or platinum (Pt). Heterogeneous catalysts comprising ruthenium (Ru) and rhenium (Re) on titania and/or zirconia supports are also disclosed. Further, disclosed are products produced by such processes, as well as products producible from such products. 1. A process for preparing a caprolactam product , the process comprising chemocatalytically converting an adipic acid substrate to a caprolactam product , wherein the step of chemocatalytically converting the adipic acid substrate to the caprolactam product comprises reacting the adipic acid substrate with hydrogen and ammonia in the presence of a heterogeneous catalyst and a solvent comprising tert-butanol.3. The process of or , wherein reacting the adipic acid substrate with hydrogen and ammonia in the presence of the heterogeneous catalyst and solvent comprises:a) combining the adipic acid substrate, the ammonia, the heterogeneous catalyst, and solvent; and,b) contacting the combined adipic acid substrate, ammonia, heterogeneous catalyst, and solvent with hydrogen.4. The process of or , wherein reacting the adipic acid substrate with hydrogen and ammonia in the presence of the heterogeneous catalyst and solvent ...

PREPARATION OF 6-AMINOCAPROIC ACID FROM ALPHA-KETOPIMELIC ACID

The invention is directed to a method for preparing 6-aminocaproic acid, comprising decarboxylating alpha-aminopimelic acid, using at least one biocatalyst comprising an enzyme having alpha-aminopimelic acid decarboxylase activity. The invention is further directed to a method for preparing caprolactam from 6-aminocaproic acid prepared by said method, to a host cell suitable for use in a method according to the invention and to a polynucleotide encoding a decarboxylase that may be used in a method according to the invention. 1. Method for preparing 6-aminocaproic acid , comprising decarboxylating alpha-aminopimelic acid , using at least one biocatalyst comprising an enzyme having alpha-aminopimelic acid decarboxylase activity , wherein said enzyme comprises an amino acid sequence selected from the group of sequences represented by any of the SEQUENCE ID NO's: 2 , 5 , 8 and 11 and homologues of said sequences having alpha-aminopimelic acid decarboxylase activity.2. Method according to claim 1 , wherein said enzyme comprises a homologue having at least 40% claim 1 , preferably at least 60% claim 1 , in particular at least 80% claim 1 , more in particular at least 90% sequence identity with any of the SEQUENCE ID NO's: 2 claim 1 , 5 claim 1 , 8 and 11.3. Method according to claim 1 , comprising preparing alpha-aminopimelic acid from alpha-ketopimelic acid.4. Method according to claim 3 , wherein the preparation of alpha-aminopimelic acid is catalysed by a biocatalyst in the presence of an amino donor claim 3 , said biocatalyst having catalytic activity with respect to the transamination or the reductive amination of alpha-ketopimelic acid.5. Method according to claim 4 , wherein the biocatalyst comprises an enzyme having catalytic activity with respect to the transamination or the reductive amination of alpha-ketopimelic acid selected from the group of aminotransferases (E.C. 2.6.1) and amino acid dehydrogenases (E.C. 1.4.1).6. Method according to claim 5 , wherein the ...

METHOD FOR PREPARING CAPROLACTAM BY USING A MICROREACTOR UNDER LEWIS ACID CATALYSIS

A method for preparing caprolactam by using a microreactor under Lewis acid catalysis, wherein a hydroxyl group in a cyclohexanone oxime is activated to obtain a cyclohexanone oxime sulfonates intermediate, then rearranged under Lewis acid catalysis to prepare the caprolactam. The method of this invention has a simple process and a high operation safety and selectivity, the reaction condition is mild, an efficient reaction can take place even at room temperature, the reaction time is short, the conversion of the cyclohexanone oxime can reach 100% within a short time, the selectivity of the caprolactam can reach 99%, the energy consumption is greatly reduced in the premise of maintaining a high yield, and the production cost is reduced, being an efficient and green and environmentally friendly method of for synthesizing the caprolactam. 1. A method for preparing caprolactam by using a microreactor under Lewis acid catalysis , comprising the following steps:(1) cyclohexanone oxime is dissolved in an organic solvent, an organic acid binding agent is added, and homogeneously mixed, to obtain a homogeneous solution;(2) a sulfonyl chlorides compound is dissolved in an organic solvent, and homogeneously mixed, to obtain a homogeneous solution;(3) a Lewis acid is dissolved in an organic solvent, and homogeneously mixed, to obtain a homogeneous solution;(4) the homogeneous solution obtained in step (1) and the homogeneous solution obtained in step (2) are concurrently and respectively pumped into a first microchannel reactor of a microreactor, and completely reacted, to obtain a cyclohexanone oxime sulphonates intermediate;(5) a mixed system obtained in step (4) and the homogeneous solution obtained in step (3) are concurrently and respectively pumped into a second microchannel reactor of the microreactor, and completely reacted, a outflow liquid is collected, to obtain the caprolactam.2. The method for preparing caprolactam by using a microreactor under Lewis acid catalysis ...

PROCESS FOR PRODUCING CYCLOHEXANONE COMPOUND

The invention has an object of providing an economical and highly efficient process for producing a cyclohexanone compound such as cyclohexanone. An aspect of the invention resides in a process for producing a cyclohexanone compound by performing hydrogenation reaction of a phenol compound in a gas phase in the presence of a palladium catalyst supported on a carrier to produce the corresponding cyclohexanone compound, wherein the hydrogenation reaction is carried out in the presence of at least one nitrogen compound selected from ammonia, amine compounds and heteroaromatic compounds. 1. A process for producing a cyclohexanone compound by performing hydrogenation reaction of a phenol compound in a gas phase in the presence of a palladium catalyst supported on a carrier to produce the corresponding cyclohexanone compound , wherein the hydrogenation reaction is carried out in the presence of at least one nitrogen compound selected from ammonia , amine compounds and heteroaromatic compounds.2. A process for producing cyclohexanone by performing hydrogenation reaction of phenol in a gas phase in the presence of a palladium catalyst supported on a carrier to produce the cyclohexanone , wherein the hydrogenation reaction is carried out in the presence of at least one nitrogen compound selected from ammonia , amine compounds and heteroaromatic compounds.3. The process for producing cyclohexanone according to claim 2 , wherein the nitrogen compound is free from a structure formed by the bonding of a hydrogen atom to a nitrogen atom.4. The process for producing cyclohexanone according to claim 3 , wherein the nitrogen compound is an amine compound having a tertiary amine structure.5. The process for producing cyclohexanone according to claim 4 , wherein the nitrogen compound is composed solely of hydrogen claim 4 , carbon and nitrogen atoms.6. The process for producing cyclohexanone according to claim 2 , wherein the nitrogen compound is the nitrogen compound attached to the ...

PROCESS FOR PREPARING LACTAMS

The present invention relates to a method for preparing lactams using heterogeneous catalysis by hydrogenating at least one compound of the following formula (I), where A is a radical of the following formula (I′) or (II′): —CH(R)—CH(R)— (I′); or —CH(R)—CH(R)—CH(R)— (II′); where R, Rand Rare, independently from each other, H, OH, an alkyl radical, or a cycloalkyl radical; and R is H or a straight or branched alkyl radical having 1 to 20, preferably 1 to 10, and more preferably 1 to 4 carbon atoms. Said method is carried out at a pressure of less than 60 bars, preferably 10 to 50 bars, in the presence of a solid hydrogenation catalyst including at least two metals selected from the group of noble metals and transition metals, and an inert substance used as a support, wherein said compound of formula (I) can be used alone or as part of a mixture. 2. The process of claim 1 , wherein the hydrogenation is carried out in the absence of solvent.3. The process of claim 1 , wherein the hydrogenation is carried out in the liquid phase.4. The process of claim 1 , wherein R claim 1 , Rand Rrepresent H or a (C-C)alkyl radical.5. The process of claim 1 , wherein A is a radical of formula —CH—CH—CH(R′)— claim 1 , and R′ represents a (C-C)alkyl radical claim 1 , and preferably methyl or ethyl.6. The process of claim 1 , wherein R is H.7. The process of claim 1 , wherein the hydrogenation is carried out at a temperature greater than or equal to 105° C.9. The process of claim 1 , wherein the pressure is between 10 bar and 50 bar.10. The process of claim 1 , wherein R represents a linear or branched alkyl radical comprising from 1 to 10 carbon atoms.11. The process of claim 1 , wherein the hydrogenation catalyst is a mixture of at least two metals selected from the group consisting of ruthenium claim 1 , platinum claim 1 , palladium claim 1 , iridium and rhodium claim 1 , said mixture being supported by an inert substance.12. The process of claim 1 , wherein the hydrogenation catalyst ...

EXTRACTION REACTOR AND ALSO METHOD FOR EXTRACTION FROM GRANULAR MATERIAL

The present disclosure relates to an extraction reactor with which granular material, in particular granular polyamide, can undergo extraction, soluble components being dissolved out of the granular material with an extraction liquid during the extraction. In the case of polyamide materials, these are for example oligomeric or monomeric components which have remained in the granular material during the polycondensation reaction for the production of the polyamide materials. 1. An extraction reactor , for liquid extraction from granular material , comprising:at least one vertically extending flow pipe including a plurality of horizontally configured heat exchanger elements that fill a cross-section of the at least one vertically extending flow pipe completely or partially and that can be flowed through by the granular material and the extraction liquid, the plurality of heat exchanger elements subdividing the at least one vertically extending flow pipe into individual vertical compartments;at least one top-side inlet for the granular material;at least one base-side outlet for the granular material;at least one base-side supply for the extraction liquid; andat least one top-side outlet for the extraction liquid.2. The extraction reactor of claim 1 , wherein at least two to thirty heat exchanger elements are present.3. The extraction reaction of claim 1 , wherein the plurality of heat exchanger elements are disposed in a vertical direction and positioned equidistant from each other claim 1 , and/or at a different spacing from each other.4. The extraction reactor of claim 1 , wherein the plurality of heat exchanger elements are selected from the group consisting of cassette bases claim 1 , baffle bases claim 1 , pipe coil constructions and combinations hereof.5. The extraction reactor of claim 4 , wherein the cassette bases comprise between nine and ninety-six individual flow elements that have respectively a separate space for the granular material and the extraction ...

METHOD FOR PRODUCING epsilon-CAPROLACTAM

The present invention is a method of producing ε-caprolactam through adipamide as an intermediate, and characteristically includes a lactamization step of reacting adipamide, formed from a material compound, with hydrogen and ammonia in the presence of a catalyst containing: a metal oxide mainly containing an oxide(s) of one or more metallic elements selected from the group consisting of metallic elements of group 5 and groups 7 to 14 in the 4th to 6th periods of the periodic table; and a metal and/or a metal compound having a hydrogenation ability. The method can increase the selectivity of ε-caprolactam. 1. A method of producing ε-caprolactam through adipamide as an intermediate , the method comprising a lactamization step of reacting adipamide , formed from a material compound , with hydrogen and ammonia in the presence of a catalyst and a solvent , wherein the catalyst comprising:a metal oxide mainly containing an oxide(s) of one or more metallic elements selected from the group consisting of metallic elements of group 5 and groups 7 to 14 in the 4th to 6th periods of the periodic table; anda metal and/or a metal compound having a hydrogenation ability.4. The method according to claim 1 , wherein the material compound is one or more carboxylic acids selected from the group consisting of adipic acid claim 1 , muconic acid claim 1 , 3-hydroxyadipic acid claim 1 , α-hydromuconic acid claim 1 , 3-hydroxyadipic acid-3 claim 1 ,6-lactone claim 1 , and muconolactone claim 1 , or a salt(s) thereof claim 1 , or a mixture thereof.5. The method according to claim 1 , wherein the oxide(s) of the metallic element(s) is/are an oxide(s) of one or more metallic elements selected from the group consisting of vanadium claim 1 , niobium claim 1 , tantalum claim 1 , manganese claim 1 , iron claim 1 , cobalt claim 1 , nickel claim 1 , copper claim 1 , zinc claim 1 , gallium claim 1 , indium claim 1 , thorium claim 1 , germanium claim 1 , tin claim 1 , and lead.6. The method ...

METHOD FOR PRODUCING OXIME

Provided is a method for efficiently producing an oxime, which is a method for producing an oxime by oxidizing, an amine, the method comprising a first contact step and a second contact step, wherein the second contact step is performed by bringing an additional amine into contact with oxygen in the presence of at least a part of an oxidation product obtained in the first contact step. 2. The method according to claim 1 , wherein the first contact step is performed in a batch manner or a semibatch manner claim 1 , and the second contact step is performed in a semibatch manner or a continuous manner.3. The method according to claim 1 , wherein the second contact step is performed in the presence of at least one catalyst selected from the group consisting of a second oxidation catalyst and a first oxidation catalyst recovered after the first contact step.4. The method according to claim 1 , wherein the first oxidation catalyst is a layered silicate.5. The method according to claim 4 , wherein the layered silicate is smectite.6. The method according to claim 4 , wherein the layered silicate contains at least one selected from the group consisting of hydrogen ions claim 4 , ammonium ions claim 4 , quaternary ammonium ions claim 4 , cations of Group 4 metal elements claim 4 , cations of Group 5 metal elements claim 4 , cations of Group 6 metal elements claim 4 , germanium ions claim 4 , positively charged oxides of Group 4 metal elements claim 4 , positively charged oxides of Group 5 metal elements claim 4 , positively charged oxides of Group 6 metal elements claim 4 , and positively charged germanium oxides.7. The method according to any one of claim 1 , wherein the oxidation product in the first contact step comprises an oxime represented by the formula (II) and a by-product claim 1 , and the second contact step is a step of further bringing at least a part of a by-product obtained in the first contact step claim 1 , the amine represented by the formula (I) claim 1 , ...

REFINING PROCESS AND REFINING SYSTEM OF CAPROLACTAM

A refining process includes steps of subjecting crude caprolactam to a first evaporative crystallization and a first solid-liquid separation to obtain a first caprolactam crystal and a first crystallization mother liquor; washing the first caprolactam crystal to obtain a second caprolactam crystal; optionally concentrating the first crystallization mother liquor to perform a second evaporative crystallization and a second solid-liquid separation to obtain a third caprolactam crystal and a second crystallization mother liquor; subjecting the third caprolactam crystal to a second washing to obtain a fourth caprolactam; optionally concentrating the second crystallization mother liquor to perform thermostatic crystallization, performing separation to obtain a fifth caprolactam crystal and a third crystallization mother liquor; washing the fifth caprolactam crystal to obtain a sixth caprolactam crystal; and subjecting the second caprolactam crystal to a hydrogenation reaction. 1. A process for refining caprolactam comprising the following steps:(1) subjecting a crude caprolactam having a caprolactam content not less than 98 wt % to a first evaporative crystallization in the presence of a first crystallization solvent, so as to obtain a first slurry;(2) subjecting the first slurry to a first solid-liquid separation to obtain a first caprolactam crystal and a first crystallization mother liquor;(3) subjecting the first caprolactam crystal to a first washing to obtain a second caprolactam crystal and a first washing liquid;(4) optionally concentrating the first crystallization mother liquor and then subjecting the concentrated first crystallization mother liquor to a second evaporative crystallization to obtain a second slurry;(5) subjecting the second slurry to a second solid-liquid separation to obtain a third caprolactam crystal and a second crystallization mother liquor;(6) subjecting the third caprolactam crystal to a second washing to obtain a fourth caprolactam and a ...

GAS AND LIQUID PHASE CATALYTIC BECKMANN REARRANGEMENT OF OXIMES TO PRODUCE LACTAMS

Methods for producing lactams from oximes by performing a Beckmann rearrangement using a silicoaluminophosphate catalyst are provided. These catalysts may be used in gas phase or liquid phase reactions to convert oximes into lactams. High conversion of oxime and high selectivity for the desired lactams are produced using the disclosed methods, including high conversion and selectivity for ε-caprolactam produced from cyclohexanone oxime and high conversion and selectivity for ω-laurolactam produced from cyclododecanone oxime. 1. A method of performing a Beckmann rearrangement reaction comprising the step of:reacting an oxime in a liquid phase in the presence of a catalyst to produce a lactam, said catalyst comprising a silicon-containing aluminophosphate with the IZA framework code FAU.2. The method of claim 1 , wherein the catalyst is a SAPO-37 catalyst.3. The method of claim 2 , wherein the catalyst is prepared from a composition having a gel loading ratio of moles of SiOto moles HPOof from 0.1:1 to 0.8:1.4. The method of claim 3 , wherein the catalyst has a silica weight percentage of from 1 wt. % to 12 wt. % of the total weight of the catalyst.5. The method of claim 2 , wherein the catalyst comprises well-isolated claim 2 , discrete Brønsted acid sites.6. The method of claim 5 , wherein the catalyst comprises an aluminophosphate framework claim 5 , the acid sites comprising silicon isomorphously substituted for phosphorous in the framework.8. The method of claim 1 , wherein said reacting step is performed at a temperature from 100° C. to 220° C.9. (canceled)10. The method of wherein said reacting step further comprises a conversion of the oxime of from 90% to 100% and a selectivity of the lactam of from 70% to 100%.11. A method of performing a Beckmann rearrangement reaction comprising the step of:reacting an oxime in a gas phase in the presence of a catalyst to produce a lactam, said catalyst comprising a silicon-containing aluminophosphates with the IZA ...

METHOD AND SYSTEM FOR PREPARING CAPROLACTAM

The present disclosure provides a method for preparing a caprolactam and the method includes steps of subjecting cyclohexanone oxime and sulfuric acid to a Beckmann rearrangement reaction to obtain a rearrangement mixture; neutralizing the rearrangement mixture and extracting the neutralized rearrangement mixture using an organic solvent sequentially; and subjecting the extracted organic solution to a hydrogenation reaction so as to simplify the process to produce a high quality caprolactam. 1. A method for preparing caprolactam , comprising steps of:(a) subjecting cyclohexanone oxime and sulfuric acid to a Beckmann rearrangement reaction to obtain a rearrangement mixture;(b) neutralizing the rearrangement mixture with an alkali to obtain a first crude caprolactam solution rich in caprolactam and a second crude caprolactam solution rich in sulfate;(c) extracting at least the first crude caprolactam solution with an organic solvent to obtain a caprolactam organic solution;{'sup': 3', '3', '2', '2, '(d) mixing the caprolactam organic solution with hydrogen to perform a hydrogenation reaction in a hydrogenation reactor having a hydrogenation catalyst, wherein a weight hourly space velocity of the caprolactam organic solution is 1 to 20 per hour, a feeding hydrogen flow rate is NM0.01 to 0.15 NMper hour per cubic meter of the caprolactam organic solution, and a hydrogen gauge pressure of an outlet of the hydrogenation reactor is 3 kg/cmto 20 kg/cm; and'}(e) purifying the hydrogenated caprolactam organic solution.2. The method according to claim 1 , further comprising extracting the second crude caprolactam solution with the organic solvent to obtain the caprolactam organic solution.3. The method according to claim 2 , wherein the first crude caprolactam solution and the second crude caprolactam solution are extracted with the organic solvent simultaneously.4. The method according to claim 1 , wherein the organic solvent is an aromatic hydrocarbon or a halogenated ...

Process for the production of a mixture comprising cyclohexanone and cyclohexanol from phenol

The present invention provides a process for continuously preparing a mixture of cyclohexanone and cyclohexanol comprising, a) hydrogenating phenol with gaseous hydrogen, in the presence of platinum or palladium, in a hydrogenation reactor, to produce a hydrogenation product stream comprising cyclohexanone, cyclohexanol, phenol and hydrogen; b) cooling the hydrogenation product stream to a temperature such that the fraction of phenol by mass in a first gas phase is lower than the fraction of phenol by mass in a first liquid phase; c) separating the first gas phase from the first liquid phase; d) returning at least part of the first gas phase to the hydrogenation reactor; e) heating the first liquid phase; f) purifying the first liquid phase by distillation; characterized in that heat is transferred from the hydrogenation product stream in step b) to another part of the process by means of in-process heat exchange; a mixture of cyclohexanone and cyclohexanol obtained by the process; and a chemical plant suitable for continuously preparing mixture of cyclohexanone and cyclohexanol according to the process.

PYRROLIDIN-2-ONE AND PIPERIDIN-2-ONE DERIVATIVES AS 11-BETA HYDROXYSTEROID DEHYDROGENASE INHIBITORS

The N-oxide forms, the pharmaceutically acceptable addition salts and the stereochemically isomeric forms thereof, wherein 2. A compound according to wherein;n is 2;{'sub': 1-3', '1-4', '1-3', '1-4', '1-4', '1-3', '1-4', '1', '1-4', '1', '1-4', '1, 'L represents a Calkyl linker optionally substituted with one or two substituents selected from Calkyl, Calkyloxy-Calkyl-, hydroxy-Calkyl, hydroxy, Calkyloxy- or phenyl-Calkyl; in particular L represents a C-linker optionally substituted with Calkyl; preferably L represents a C-linker substituted with Calkyl, more preferably a C-linker substituted with methyl;'}{'sub': 1-2', '1-4', '1-4', '1', '1-4, 'M represents a direct bond or a Calkyl optionally substituted with one or two substituents selected from hydroxy, Calkyl or Calkyloxy-; preferably M represents a C-linker optionally substituted with Calkyl;'}{'sup': '1', 'sub': 1-4', '1-4', '1-4, 'Rrepresents hydrogen, hydroxy, halo, Calkyl, Calkyloxy-, or Calkyloxy substituted with halo;'}{'sup': 2', '1, 'sub': 1-4', '1-4', '1-4, 'Rrepresents hydrogen, halo, Calkyl, Calkyloxy- or Ar—Calkyloxy-;'}{'sup': '3', 'sub': 1-4', '1-4, 'Rrepresents hydrogen, halo, Calkyl, Calkyloxy- or cyano;'}{'sup': '4', 'sub': 1-4', '1-4, 'Rrepresents hydrogen, halo, Calkyl or Calkyloxy-;'}{'sup': 5', '2, 'sub': 1-4', '1-4, 'Rrepresents hydrogen, Calkyl or Ar—Calkyl; in particular hydrogen;'}{'sup': '6', 'sub': '1-4', 'Rrepresents hydrogen, halo, or Calkyloxy; in particular hydrogen, chloro, fluoro, bromo or methoxy;'}{'sup': '1', 'Arrepresents phenyl;'}{'sup': '2', 'Arrepresents phenyl or naphtyl.'}3. (canceled)4. A compound according to wherein Ris at the para position claim 1 , L represents a C-alkyl linker and M represents a C-linker.5. A compound according to wherein L represents a C-linker substituted with a Calkyl claim 1 , CalkyloxyCalkyl- claim 1 , hydroxyCalkyl- or phenylCalkyl- wherein said Calkyl claim 1 , CalkyloxyCalkyl- claim 1 , hydroxyCalkyl- or phenylCalkyl- is in the S- ...

GLYCOLACTAM COMPOUNDS, PROCESS FOR PREPARATION AND USES THEREOF

The present invention discloses compounds of Formula I, Wherein, R═R═R═R═R═R═R═Rand is selected from H, OBn, OH, CHOH, CHOH, CH; Ris selected front alkyl, substituted alkyl, hydroxyl alkyl, alkenyl, benzyl; process for preparation of N-alkylated glycolactain compounds of Formula I and their use for the synthesis of piperidine alkaloids and their analogues. 19-. (canceled)12. The compound as claimed in claim 10 , wherein said compound is:(4R,5R,6R)-4,5-bis(benzyloxy)-6-((benzyloxy)methyl)-1-methylpiperidin-2-one(3a);(4R,5S,6R)-4,5-bis(benzyloxy)-6-((benzyloxy)methyl)-1-methylpiperidin-2-one(4a);(4R,5S,6R)-4,5-bis(benzyloxy)-6-((benzyloxy)methyl)-1-ethylpiperidin-2-one(5a);(4R,5S,6R)-4,5-bis(benzyloxy)-6-((benzyloxy)methyl)-1-ethylpiperidin-2-one(6a);(4R,5R,6R)-4,5-bis(benzyloxy)-6-((benzyloxy)methyl)-1-propyl piperidine-2-one(7 a);(4R,5R,6R)-4,5-bis(benzyloxy)-6-((benzyloxy)methyl)-1-propylpiperidin-2-one(8a);(4R,5R,6R)-4,5-bis(benzyloxy)-6-((benzyloxy)methyl)-1-butylpiperidin-2-one(9a);(4R,5S,6R)-4,5-bis(benzyloxy)-6-((benzyloxy)methyl)-1-butylpiperidin-2-one(10a);(4R,5R,6R)-1-benzyl-4,5-bis(benzyloxy)-6-((benzyloxy)methyl)piperidin-2-one(11a);(4R,5R,6R)-1-allyl-4,5-bis(benzyloxy)-6-((benzyloxy)methyl)piperidin-2-one(12a);(4R,5S,6R)-1-allyl-4,5-bis(benzyloxy)-6-((benzyloxy)methyl)piperdin-2-one(13a);(4R,5R,6R)-4,5-bis(benzyloxy)-1-(2-(benzyloxy)ethyl)-6-((benzyloxy)methyl)piperidin-2-one(14a);(4R,5S,6R)-4,5-bis(benzyloxy)-1-(2-(benzyloxy)ethyl)-6-((benzyloxy)methyl)piperidin-2-one(15a);(5S,6R)-5-(benzyloxy)-6-((benzyloxy)methyl)-1-methyl-5,6-dihydropyridin-2(1H)-one (16b);(5R,6R)-5-(benzyloxy)-6-((benzyloxy)methyl)-1-methyl-5,6-dihydropyridin-2(1H)-one(17b);(5S,6R)-5-(benzyloxy)-6-((benzyloxy)methyl)-1-ethyl-5,6-dihydropyridin-2(1H)-one(18b);(5R,6R)-5-(benzyloxy)-6-((benzyloxy)methyl)-1-ethyl-5,6-dihydropyridin-2(1H)-one(19b);(5S,6R)-5-(benzyloxy)-6-(benzyloxy)methyl)-1-propyl-5,6-dihydropyridin-2(1H)-one(20b);(5R,6R)-5-(benzyloxy)-6-((benzyloxy)methyl)-1-propyl-5,6 ...

Process for Separating Methylcyclopentanone from Cyclohexanone

In a process for separating methylcyclopentanone from a mixture comprising methylcyclopentanone and cyclohexanone, a feedstock comprising cyclohexanone, methylcyclopentanone, water at a concentration of at least 0.10 wt %, and optionally phenol is fed into a fractionation distillation column, where a lower effluent rich in cyclohexanone and an upper effluent rich in methylcyclopentanone are produced. Due to the inclusion of water at a relatively high concentration in the feedstock, efficient separation of methylcyclopentanone is achieved. In certain particularly desirable embodiments, the lower effluent is substantially free of methylcyclopentanone. The thus produced cyclohexanone may be used to make, e.g., high-purity caprolactam, which, in turn, may be used for fabricating, e.g., high-performance nylon-6 material. 1. A process for separating methylcyclopentanone from a mixture comprising cyclohexanone and methylcyclopentanone , the process comprising:(I) providing a first feedstock comprising cyclohexanone and methylcyclopentanone, the methylcyclopentanone having a concentration CMCP(1);(II) including water in the first feedstock at a concentration CH2O(1) of at least 0.10 wt %; and(III) fractionating the first feedstock in a first distillation column to obtain a first upper effluent rich in methylcyclopentanone having a methylcyclopentanone concentration of CMCP(2) and a first lower effluent rich in cyclohexanone, wherein CMCP(2)/CMCP(1)≧3.0.2. The process according to claim 1 , wherein the first distillation column comprises N theoretical trays claim 1 , where 1≦N≦80.3. The process according to claim 1 , wherein CMCP(2)/CMCP(1)≧20.0.4. The process according to claim 1 , wherein the first lower effluent has a methylcyclopentanone concentration CMCP(3) claim 1 , and CMCP(1)/CMCP(3)≧10.0.5. The process according to claim 1 , wherein the first lower effluent has a methylcyclopentanone concentration of less than 20 ppm.6. The process according to claim 1 , wherein ...

METHOD AND SYSTEM FOR PREPARING CAPROLACTAM

The present disclosure provides a method for preparing a caprolactam and the method includes steps of subjecting cyclohexanone oxime and sulfuric acid to a Beckmann rearrangement reaction to obtain a rearrangement mixture; neutralizing the rearrangement mixture and extracting the neutralized rearrangement mixture using an organic solvent sequentially; and subjecting the extracted organic solution to a hydrogenation reaction so as to simplify the process to produce a high quality caprolactam. 1. A method for preparing caprolactam , comprising steps of:(a) subjecting cyclohexanone oxime and sulfuric acid to a Beckmann rearrangement reaction to obtain a rearrangement mixture;(b) neutralizing the rearrangement mixture with an alkali to obtain a first crude caprolactam solution rich in caprolactam and a second crude caprolactam solution rich in sulfate;(c) extracting at least the first crude caprolactam solution with an organic solvent to obtain a caprolactam organic solution;{'sup': 3', '3', '2', '2, '(d) mixing the caprolactam organic solution with hydrogen to perform a hydrogenation reaction in a hydrogenation reactor having a hydrogenation catalyst, wherein a weight hourly space velocity of the caprolactam organic solution is 1 to 20 per hour, a feeding hydrogen flow rate is NM0.01 to 0.15 NMper hour per cubic meter of the caprolactam organic solution, and a hydrogen gauge pressure of an outlet of the hydrogenation reactor is 3 kg/cmto 20 kg/cm; and'}(e) purifying the hydrogenated caprolactam organic solution.2. The method according to claim 1 , further comprising extracting the second crude caprolactam solution with the organic solvent to obtain the caprolactam organic solution.3. The method according to claim 2 , wherein the first crude caprolactam solution and the second crude caprolactam solution are extracted with the organic solvent simultaneously.4. The method according to claim 1 , wherein the organic solvent is an aromatic hydrocarbon or a halogenated ...

THREE-PHASE AC/DC CONVERTER, PHOTOCHEMICAL REACTION DEVICE AND METHOD USING SAME, AND METHOD FOR PRODUCING LACTAM

Provided are a three-phase AC/DC converter disposed between a three-phase AC power supply and a light emitting diode group, the converter including a three-phase full bridge circuit in which pairs of switching elements are connected in parallel between DC buses for the three phases of the three-phase AC power supply; reactors connecting connection portions between the switching elements and corresponding phases of the three-phase AC power supply; a smoothing capacitor on the output side of the three-phase full bridge circuit; a DC voltage detection means; a power supply voltage phase detection means; and a pulse width modulation means for outputting pulse width modulation signals of the switching elements, wherein the pulse width modulation means outputs the pulse width modulation signals based on a power supply voltage phase and an output voltage between the DC buses. 1. A three-phase AC/DC converter incorporated into a power supply circuit disposed between a three-phase AC power supply and a light emitting diode group , in order to drive said light emitting diode group of 3 kw or more with a single unit , said converter comprising:DC buses connected to said light emitting diode group;a three-phase full bridge circuit in which pairs of switching elements, in each of which a pair of switching elements are connected in series, are connected in parallel between said DC buses by pairs for three phases of said three-phase AC power supply, and each switching element has a reverse-blocking diode connected thereto in parallel;a reactor provided between said three-phase full bridge circuit and said three-phase AC power supply for connecting a connection portion between switching elements in said each pair of switching elements and a corresponding phase of said three-phase AC power supply;a smoothing capacitor connected between said DC buses on an output side of said three-phase full bridge circuit;a DC voltage detection means for detecting an output voltage between said DC ...

Biological Synthesis of 6-Aminocaproic Acid and Transgenic Microorganism Therefor

The present invention relates to a method for preparing a recombinant microorganism simultaneously comprising genes encoding enzymes used in the biosynthesis pathway of 6-aminocaproic acid, which is a precursor of caprolactam, biosynthesizing 6-aminocaproic acid from the microorganism, and producing the same so as to synthesize caprolactam. 1. A method for preparing 6-aminocaproic acid comprising:preparing an expression vector comprising HpaI (4-hydroxy-2-oxoheptane-1,7-dioate aldolase)-HpaH (2-oxohept-3-ene-1,7-dioate dehydratase) gene, nemA (N-ethylmaleimide reductase) gene, and KIVD (alpha-ketoisovalerate decarboxylase) gene; and at least one of PdAT (beta-alanine-pyruvate transaminase) gene and BcAT (adenosylmethionine-8-amino-7-oxononanoate aminotransferase) gene (step 1); andtransforming the expression vector of step 1 into a microorganism (step 2).2. The method of claim 1 , wherein the HpaI-HpaH gene comprises a polynucleotide represented by SEQ ID NO: 3 encoding aldolase-dehydratase.3. The method of claim 1 , wherein the nemA gene comprises a polynucleotide represented by SEQ ID NO: 4 encoding reductase.4. The method of claim 1 , wherein the KIVD (alpha-ketoisovalerate decarboxylase) gene comprises a polynucleotide represented by SEQ ID NO: 5 encoding decarboxylase.5. The method of claim 1 , wherein the PdAT (beta-alanine-pyruvate transaminase) gene comprises a polynucleotide represented by SEQ ID NO: 6 encoding transaminase.6. The method of claim 1 , wherein BcAT (adenosylmethionine-8-amino-7-oxononanoate aminotransferase) gene comprises a polynucleotide represented by SEQ ID NO: 7 encoding transaminase.7. The method of claim 1 , wherein the expression vector of step 1 further comprises nucleic acid (polynucleotide) sequences encoding GST claim 1 , MBP claim 1 , NusA claim 1 , thioredoxin claim 1 , ubiquitin claim 1 , FLAG claim 1 , BAP claim 1 , 6H15 claim 1 , STREP claim 1 , CBP claim 1 , CBD claim 1 , or S-tag affinity tag.8. The method of claim 1 , ...

PROCESSES OF MAKING AND CRYSTALLINE FORMS OF A MDM2 INHIBITOR

The present invention provides processes for making 2-((3R,5R,6S)-5-(3-chlorophenyl)-6-(4-chlorophenyl)-1-((S)-1-(isopropylsulfonyl)-3-methylbutan-2-yl)-3-methyl-2-oxopiperidin-3-yl)acetic acid as well as intermediates and processes for making the intermediates. Also provided are crystalline forms of the compound and the intermediates. 238.-. (canceled) The present invention provides processes for making 2-((3R,5R,6S)-5-(3-chlorophenyl)-6-(4-chlorophenyl)-1-((S)-1-(isopropylsulfonyl)-3-methylbutan-2-yl)-3-methyl-2-oxopiperidin-3-yl)acetic acid (“Compound A” herein) as well as intermediates and processes for making the intermediates. Also provided are crystalline forms of the compound and the intermediates.p53 is a tumor suppressor and transcription factor that responds to cellular stress by activating the transcription of numerous genes involved in cell cycle arrest, apoptosis, senescence, and DNA repair. Unlike normal cells, which have infrequent cause for p53 activation, tumor cells are under constant cellular stress from various insults including hypoxia and pro-apoptotic oncogene activation. Thus, there is a strong selective advantage for inactivation of the p53 pathway in tumors, and it has been proposed that eliminating p53 function may be a prerequisite for tumor survival. In support of this notion, three groups of investigators have used mouse models to demonstrate that absence of p53 function is a continuous requirement for the maintenance of established tumors. When the investigators restored p53 function to tumors with inactivated p53, the tumors regressed.p53 is inactivated by mutation and/or loss in 50% of solid tumors and 10% of liquid tumors. Other key members of the p53 pathway are also genetically or epigenetically altered in cancer. MDM2, an oncoprotein, inhibits p53 function, and it is activated by gene amplification at incidence rates that are reported to be as high as 10%. MDM2, in turn, is inhibited by another tumor suppressor, p14ARF. It has ...

PROCESSES OF MAKING AND CRYSTALLINE FORMS OF A MDM2 INHIBITOR

The present invention provides processes for making 2-((3R,5R,6S)-5-(3-chlorophenyl)-6-(4-chlorophenyl)-1-((S)-1-(isopropylsulfonyl)-3-methylbutan-2-yl)-3-methyl-2-oxopiperidin-3-yl)acetic acid as well as intermediates and processes for making the intermediates. Also provided are crystalline forms of the compound and the intermediates. 122.-. (canceled)25. The process of wherein the base is sodium tert-butoxide.26. The process of wherein the oxidation is accomplished using RuCland NaIO.2938.-. (canceled) The present invention provides processes for making 2-((3R,5R,6S)-5-(3-chlorophenyl)-6-(4-chlorophenyl)-1-((S)-1-(isopropylsulfonyl)-3-methylbutan-2-yl)-3-methyl-2-oxopiperidin-3-yl)acetic acid (“Compound A” herein) as well as intermediates and processes for making the intermediates. Also provided are crystalline forms of the compound and the intermediates.p53 is a tumor suppressor and transcription factor that responds to cellular stress by activating the transcription of numerous genes involved in cell cycle arrest, apoptosis, senescence, and DNA repair. Unlike normal cells, which have infrequent cause for p53 activation, tumor cells are under constant cellular stress from various insults including hypoxia and pro-apoptotic oncogene activation. Thus, there is a strong selective advantage for inactivation of the p53 pathway in tumors, and it has been proposed that eliminating p53 function may be a prerequisite for tumor survival. In support of this notion, three groups of investigators have used mouse models to demonstrate that absence of p53 function is a continuous requirement for the maintenance of established tumors. When the investigators restored p53 function to tumors with inactivated p53, the tumors regressed.p53 is inactivated by mutation and/or loss in 50% of solid tumors and 10% of liquid tumors. Other key members of the p53 pathway are also genetically or epigenetically altered in cancer. MDM2, an oncoprotein, inhibits p53 function, and it is activated ...

SYNTHESIS OF LACTAM BASED IONIC LIQUID

Lactamium based ionic liquids are described. They comprise at least one of: 2. The ionic liquid of wherein the lactam compound has the general formula (I).3. The ionic liquid of wherein the lactam compound has the general formula (II).4. The ionic liquid of wherein an anion of the Brønsted acid HX is at least one of: carboxylates claim 3 , nitrates claim 3 , phosphates claim 3 , phosphinates claim 3 , phosphonates claim 3 , imides claim 3 , cyanates claim 3 , borates claim 3 , sulfates claim 3 , sulfonates claim 3 , acetates claim 3 , and halides.5. The ionic liquid of wherein the lactam compound has the general formula (III).6. The ionic liquid of wherein an anion of the Brønsted acid HX is at least one of: carboxylates claim 1 , nitrates claim 1 , phosphates claim 1 , phosphinates claim 1 , phosphonates claim 1 , imides claim 1 , cyanates claim 1 , borates claim 1 , sulfates claim 1 , sulfonates claim 1 , acetates claim 1 , and halides.7. The ionic liquid of wherein at least one of the rings has at least one double bond.9. The method of wherein the lactam compound has the general formula (IV).10. The method of wherein the lactam compound has the general formula (V).11. The method of wherein the Brønsted acid HX is at least one of sulfuric acid claim 10 , p-toluenesulfonic acid claim 10 , hydrochloric acid claim 10 , hydrobromic acid claim 10 , nitric acid claim 10 , phosphoric acid claim 10 , tetrafluoroboric acid claim 10 , triflic acid claim 10 , trifluoroacetic acid claim 10 , chloroacetic acid claim 10 , and methanesulfonic acid.12. The method of wherein an anion of the Brønsted acid HX is at least one of carboxylates claim 10 , nitrates claim 10 , phosphates claim 10 , phosphinates claim 10 , phosphonates claim 10 , imides claim 10 , cyanates claim 10 , borates claim 10 , sulfates claim 10 , sulfonates claim 10 , acetates claim 10 , and halides.13. The method of wherein the lactam compound has the general formula (VI).14. The method of wherein the Brønsted ...

PROCESS FOR PREPARING INTERMEDIATE OF ANTI-TUMOR DRUG NIRAPARIB AND INTERMEDIATE THEREOF

Disclosed is a process for preparing an intermediate of anti-tumor drug niraparib and an intermediate thereof. The present invention discloses a process for preparing compound f, which comprises conducting a cyclization reaction of compound e in a solvent and in the presence of a base to give compound f. The process of the present invention does not involve the steps of catalytic reduction or catalytic coupling reaction of precious metals and chiral separation, which has advantages such as low equipment requirements, simple operation, favorable industrial production, avoiding waste liquid containing heavy metals and phosphorus, low cost and high product ee value. 7. The process for preparing compound f as defined in claim 6 , wherein claim 6 , further comprising a recrystallization treatment after completion of the cyclization reaction; the solvent for recrystallization is an ethers solvent claim 6 , a nitriles solvent claim 6 , an esters solvent claim 6 , a mixed solvent of an ethers solvent and an alkanes solvent claim 6 , a mixed solvent of a nitriles solvent and an alkanes solvent claim 6 , or a mixed solvent of an esters solvent and an alkanes solvent.9. The process for preparing compound f as defined in claim 8 , wherein claim 8 , in the process for preparing compound e claim 8 , the solvent is a haloalkanes solvent and/or an esters solvent claim 8 , preferably dichloromethane and/or isopropyl acetateand/or, the condensing agent is N,N′-carbonyldiimidazole or 2-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate.10. The process for preparing compound f as defined in claim 8 , wherein claim 8 , the process for preparing compound e comprises mixing a mixed solution of the acidic salt of compound c or compound c claim 8 , compound d and the solvent claim 8 , and a mixed solution of the condensing agent and the solvent at −5 to 5° C. to conduct the reaction claim 8 , preferably claim 8 , the mixed solution of the condensing agent and the ...

METHOD FOR PRODUCING EPSILON-CAPROLACTAM

The present invention relates to a method of producing ε-caprolactam, the method including the following steps (A) and (B): (A) a step of reacting 5-cyanovaleramide with hydrogen in an aqueous solvent in a presence of a hydrogenation catalyst to obtain a 5-cyanovaleramide hydrogenation reaction mixture; (B) a step of heating the 5-cyanovaleramide hydrogenation reaction mixture at a temperature of 180° C. or higher and 300° C. or lower in an aqueous solvent to obtain ε-caprolactam. 1. A method of producing ε-caprolactam , the method comprising the following steps (A) and (B):(A) a step of reacting 5-cyanovaleramide with hydrogen in an aqueous solvent in a presence of a hydrogenation catalyst to obtain a 5-cyanovaleramide hydrogenation reaction mixture;(B) a step of heating the 5-cyanovaleramide hydrogenation reaction mixture at a temperature of 180° C. or higher and 300° C. or lower in an aqueous solvent to obtain ε-caprolactam.2. The method according to claim 1 , wherein the step (A) is performed in an absence of ammonia.3. The method according to claim 1 , wherein a reaction temperature in the step (A) is 50° C. or higher and 200° C. or lower.4. The method according to claim 1 , wherein the temperature of the step (B) is 200° C. or higher and lower than 280° C.5. The method according to claim 1 , wherein the step (B) is performed in an absence of a catalyst.6. The method according to claim 1 , wherein a ratio of 6-aminocaproic acid amide contained in the 5-cyanovaleramide hydrogenation reaction mixture is 45 mol % or more and 72 mol % or less.7. (canceled)8. An ε-caprolactam composition having a ratio of 6-aminocaproic acid amide to ε-caprolactam of 0.1 mol % or more and 5 mol % or less claim 1 , and comprising no ammonia. The present invention relates to a method of producing ε-caprolactam that is a raw material for a polyamide.ε-Caprolactam is an important chemical raw material that is a raw material for a polyamide and is industrially produced all over the world ...

PROCEDURE FOR OBTAINING CAPROLACTAMA.

FABRICACION DE CAPROLACTAMA MEDIANTE TRANSFORMACION DE 6 AMINOCAPRONITRILO CON AGUA EN PRESENCIA DE CATALIZADORES, EMPLEANDO UNA MEZCLA DE BASE DE 6 TETRAHIDROAZEPINA DE LA FORMULA (I), Y TRANSFORMACION EN LA FASE LIQUIDA EN PRESENCIA DE CATALIZADORES HETEROGENEOS, ASI COMO PROCEDIMIENTO PARA LA FABRICACION DEL DERIVADO DE TETRAHIDROAZEPINA (I) Y SU EMPLEO PARA LA FABRICACION DE CAPROLACTAMA Y POLICAPROLACTAMA. MANUFACTURING OF CAPROLACTAMA THROUGH TRANSFORMATION OF 6 AMINOCAPRONITRILE WITH WATER IN THE PRESENCE OF CATALYZERS, USING A BASE MIXTURE OF 6 TETRAHYDROAZEPIN OF FORMULA (I), AND TRANSFORMATION IN THE LIQUID PHASE IN THE PRESENCE OF CATALYZERS AS FITTING THE DEVELOPMENTS OF TETRAHYDROAZEPIN (I) AND ITS EMPLOYMENT FOR THE MANUFACTURE OF CAPROLACTAMA AND POLICAPROLACTAMA.

Methods and compositions for using non-ionic contrast agents to reduce the risk of clot formation in diagnostic procedures

In accordance with the present invention a novel method and composition for using nonionic contrast media to reduce the risk of clot formation in a diagnostic procedure is disclosed. Novel compositions for such method are also disclosed. The present method comprises employing a triiodinated phenyl contrast agent having a heterocyclic group or a dimeric triiodinated phenyl contrast agent having one or more heterocyclic groups.

Production method of caprolactam

본 발명은 6-아미노카프로니트릴과 하기 화학식 I의 테트라히드로아제핀 유도체의 출발 혼합물을 사용하여 촉매의 존재 하에서 6-아미노카프로니트릴과 물의 반응에 의한 카프로락탐의 생산, 불균일 촉매 존재 하에서의 액상 반응 및 테트라히드로아제핀 유도체 I의 제조 방법 및 카프로락탐과 폴리카프로락탐을 제조하기 위한 그의 용도를 기술한다. The present invention relates to the production of caprolactam by reaction of 6-aminocapronitrile with water in the presence of a catalyst using a starting mixture of 6-aminocapronitrile and a tetrahydroazepine derivative of the formula (I), a liquid phase reaction in the presence of a heterogeneous catalyst and Processes for the preparation of tetrahydroazepine derivatives I and their use for preparing caprolactam and polycaprolactam are described. <화학식 I> (I)

Biochemical synthesis of 6-amino caproic acid

Method for directly synthesizing caprolactam from cyclohexanone serving as raw material

本发明为一种以环己酮为原料直接合成己内酰胺的方法，该方法包括以下步骤：将环己酮、离子液体型羟胺盐和锌盐催化剂加入反应器中，加入溶剂，搅拌、回流冷凝，在常压、50~90℃下反应1~5h，得产物己内酰胺；所述的离子液体型羟胺盐为1-磺丁基-3-甲基咪唑硫酸氢盐离子液体型羟胺盐。本发明在同一个反应器中，实现了环己酮和羟胺合成环己酮肟、以及环己酮肟重排制备己内酰胺两步反应的集成，缩短了反应流程，节省了设备投资；反应条件温和；不副产低价值的硫酸铵；环己酮的转化率和己内酰胺的选择性很高，最高可以达到82.7%和97.5%。

Device and method for treating hydrogenation tail gas

本发明公开了一种处理加氢尾气的装置及方法，包括用于将氢气和己内酰胺充分混合反应的反应罐，所述反应罐左侧设有用于加料的加料组件，所述反应罐内部设有用于收集反应后液体的集液池，所述集液池所在的反应罐内壁设有用于检测液位高度的液位传感器，所述反应罐的出料端连接用于存储物料的成品收集箱，所述成品收集箱上端的排气口与气液分离器的进气端连接，本发明针对现有装置的弊端进行设计，通过对固体物料进行加热液化，从而实现液封处理，防止了空气的进入，另外通过构建混合反应件使得氢气与雾化液体充分混合，构建多层由内到外的压缩性环状腔室，从而使得物料充分反应，减少了氢气的用量，使得后期尾气处理难度降低，实用性强。

A-cycloalkylbenzyl lactamimides

Bleach composition comprising N-acylcaprolactam activator

Bleaching compounds comprising substituted benzoyl caprolactam bleach activators

提供了含有取代的苯甲酰基己内酰胺漂白活化剂的衣物洗涤剂和漂白体系。漂白活化剂对混合的污渍有效，特别是对疏水和亲水污垢和污渍混合物有效。

Bleaching compounds comprising acyl valerolactam bleach activators

Laundry detergents and bleaching systems comprise acyl valerolactam bleach activators. The bleach activators are effective under mixed soil conditions, especially mixtures of hydrophobic and hydrophilic soils and stains.

Bleaching activators

用作漂白活化剂以及新的过羧酸的新化合物包含含氮杂环基团，该活化剂与过氧漂白源在水溶液中反应后生成中间体。优选的活化剂是二元羧酸的对称的衍生物，有N，N′二酰基N-杂环基，通常为内酰胺的衍生物。它们由2摩尔内酰胺与1摩尔二元酰基氯或酐反应制得。

A kind of effectively refining method of caprolactam

本发明公开了一种己内酰胺的高效精制方法，本方法是重排反应生产己内酰胺过程中的重排反应产物经过闪蒸、离心分离、蒸发蒸馏、膜过滤和结晶等简单操作，即可得到符合工业要求的高纯度己内酰胺成品和尼龙切片产品。本发明适用于气相、液相和溶剂重排等方法所得反应物的精制，应用范围广泛；采用本发明技术，与传统己内酰胺提纯工艺相比，可制备出品质较高的己内酰胺产品，中间产物己内酰胺晶体又可制备成尼龙切片产品，且在一定程度上缩短了生产流程，显著减少了溶剂用量和废水排放，大大降低了投资和生产成本。

A kind of preparation method of caprolactam and N substitution caprolactams

本发明提出了一种己内酰胺及N取代己内酰胺的制备方法，包括以下步骤：加入催化剂：在固定床中装入Φ＝4.0～6.0mm的颗粒型SO 4 2‑ /M x O y 类固体超强酸催化剂150.0～200.0g，加热：加热使温度升到180.0～320.0℃，通入氮气：以空速50.0～70.0cm 3 /min向固定床通入氮气，使催化剂始终处于氮气保护状态，该制备方法以6‑己内酯和氨(胺)为原料，在常压及氮气保护下将原料气化后通过装有固体超强酸催化剂的固定床进行反应，产物经冷凝收集、脱水脱溶剂得到高纯度的己内酰胺及N取代己内酰胺，收率达95％以上，其催化工艺简单，产品收率及纯度高，成本低、可连续化生产，十分有利于工业化生产。

Amine salt of organic peroxide and use

(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。

Method for preparing epsilon-caprolactam

FIELD: organic chemistry, chemical technology. SUBSTANCE: invention relates to technology for preparing caprolactam by the cyclization reaction of derivatives of aminocaproic acid. Method is carried out by cyclizing hydrolysis of compound chosen from the group comprising aminocaproic acid esters or amides, or their mixtures. The process is carried out in the presence of water, in vapor phase at temperature 200-450°C in the presence of a solid catalyst comprising of aluminum oxide that comprises at least one macroporosity with pores volume corresponding to pores with diameter above 500 Å taken in the concentration 5 ml/100 g of above. Preferably, the specific square of catalyst particles is above 10 m 2 /g and the total volume of pores is 10 ml/100 g or above wherein pores volume corresponds to pores with diameter above 500 Å is 10 ml/100 g or above. Invention provides improving the process indices due to the improved properties of the solid catalyst. EFFECT: improved preparing method. 5 cl, 2 ex ÐÎÑÑÈÉÑÊÀß ÔÅÄÅÐÀÖÈß RU (19) (11) 2 275 358 (13) C2 (51) ÌÏÊ C07D 201/08 (2006.01) C07D 223/10 (2006.01) B01J 21/04 (2006.01) B01J 35/04 (2006.01) ÔÅÄÅÐÀËÜÍÀß ÑËÓÆÁÀ ÏÎ ÈÍÒÅËËÅÊÒÓÀËÜÍÎÉ ÑÎÁÑÒÂÅÍÍÎÑÒÈ, ÏÀÒÅÍÒÀÌ È ÒÎÂÀÐÍÛÌ ÇÍÀÊÀÌ (12) ÎÏÈÑÀÍÈÅ ÈÇÎÁÐÅÒÅÍÈß Ê ÏÀÒÅÍÒÓ (21), (22) Çà âêà: 2004122428/04, 13.12.2002 (72) Àâòîð(û): ËÅÊÎÍÒ Ôèëèïï (FR) (24) Äàòà íà÷àëà îòñ÷åòà ñðîêà äåéñòâè ïàòåíòà: 13.12.2002 (73) Ïàòåíòîîáëàäàòåëü(è): ÐÎÄÈÀ ÏÎËÈÀÌÈÄ ÈÍÒÅÐÌÅÄÈÝÉÒÑ (FR) (30) Ïðèîðèòåò: 21.12.2001 FR 0116659 R U (43) Äàòà ïóáëèêàöèè çà âêè: 10.05.2005 (45) Îïóáëèêîâàíî: 27.04.2006 Áþë. ¹ 12 2 2 7 5 3 5 8 (56) Ñïèñîê äîêóìåíòîâ, öèòèðîâàííûõ â îò÷åòå î ïîèñêå: US 3658810 À, 25.04.1972. RU 2151765 Ñ1, 27.06.2000. RU 2118315 Ñ1, 27.08.1998. WO 97/30973 À1, 28.08.1997. (85) Äàòà ïåðåâîäà çà âêè PCT íà íàöèîíàëüíóþ ôàçó: 21.07.2004 2 2 7 5 3 5 8 R U (87) Ïóáëèêàöè PCT: WO 03/053935 (03.07.2003) C 2 C 2 (86) Çà âêà PCT: FR 02/04344 (13.12.2002) Àäðåñ äë ïåðåïèñêè: 129010, Ìîñêâà, óë. Á.Ñïàññêà ...

Production of epsilon-caprolactam over high-silica zeolite nanosheets

본 발명은 고 실리카 나노판상형 제올라이트를 이용한 ε-카프로락탐의 제조방법을 제공한다. 본 발명의ε-카프로락탐의 제조방법은, 기상 베크만 전환 공정을 이용하여 시클로헥사논 옥심으로부터 ε-카프로락탐을 제조하는 방법에 있어서, 단일 단위 결정 격자 한 개 또는 10 개 이하가 연결되어 규칙적이거나 불규칙적으로 배열된 다중 또는 단일 판상 구조의 제올라이트 물질을 촉매로 사용하는 것을 특징으로 한다. 본 발명의 ε-카프로락탐 제조 방법에 의하면, 높은 옥심의 전환율, 높은 ε-카프로락탐 선택성, 매우 느린 촉매의 비활성화 특성을 갖는 고 실리카 나노판상형 제올라이트를 이용함으로써, ε-카프로락탐의 생산성을 비약적으로 증진시킬 수 있다. 아울러, 기존의 잦은 촉매 교체 및 재생 과정 또한 크게 줄일 수 있어, 보다 경제적이고 효율적으로 ε-카프로락탐을 제조할 수 있다. The present invention provides a method for producing ε-caprolactam using high silica nanoplatelet zeolite. The method for producing ε-caprolactam of the present invention is a method for producing ε-caprolactam from cyclohexanone oxime using a gas phase Beckman conversion process, in which one single crystal lattice or ten or less are connected to be regular or Irregularly arranged multi- or single-plate zeolite materials are used as catalysts. According to the method for producing ε-caprolactam of the present invention, the productivity of ε-caprolactam is dramatically increased by using a high silica nanoplatelet zeolite having high oxime conversion, high ε-caprolactam selectivity, and very slow catalyst deactivation characteristics. Can be promoted. In addition, the existing frequent catalyst replacement and regeneration process can also be greatly reduced, making it possible to manufacture ε-caprolactam more economically and efficiently.

The method of separating-purifying N- methyl caprolactam from the light impurity component of cyclohexanone oxime gas phase beckmann rearrangement product

本发明公开了一种从环己酮肟气相贝克曼重排产物的轻杂质组分中分离提纯N‑甲基己内酰胺的方法。该方法包括：1)将所述轻杂质组分进行蒸馏分离，得到塔底馏分；2)在所述塔底馏分中加入含水无机酸以中和苯胺及其同系物，形成溶于水的铵盐；3)在2)所得到的混合物中加入有机溶剂和可选的水进行萃取，以分离溶解在水相中的铵盐；4)在3)所得到的有机相中加入水进行多次萃取以分离溶解在水相中的N‑甲基己内酰胺，得到N‑甲基己内酰胺水溶液；5)对所述N‑甲基己内酰胺水溶液进行蒸发处理，得到所述N‑甲基己内酰胺。应用本发明所提供这种方法，可以得到高纯度的N‑甲基己内酰胺，可以提高气相重排工艺的经济性。

Patent JPS5012076A

METHOD FOR PRODUCING LACTAM

ÐÎÑÑÈÉÑÊÀß ÔÅÄÅÐÀÖÈß (19) RU (51) ÌÏÊ 7 (11) (13) 2004 122 428 A C 07 D 223/10 ÔÅÄÅÐÀËÜÍÀß ÑËÓÆÁÀ ÏÎ ÈÍÒÅËËÅÊÒÓÀËÜÍÎÉ ÑÎÁÑÒÂÅÍÍÎÑÒÈ, ÏÀÒÅÍÒÀÌ È ÒÎÂÀÐÍÛÌ ÇÍÀÊÀÌ (12) ÇÀßÂÊÀ ÍÀ ÈÇÎÁÐÅÒÅÍÈÅ (21), (22) Çà âêà: 2004122428/04, 13.12.2002 (71) Çà âèòåëü(è): ÐÎÄÈÀ ÏÎËÈÀÌÈÄ ÈÍÒÅÐÌÅÄÈÝÉÒÑ (FR) (30) Ïðèîðèòåò: 21.12.2001 FR 0116659 (72) Àâòîð(û): ËÅÊÎÍÒ Ôèëèïï (FR) (85) Äàòà ïåðåâîäà çà âêè PCT íà íàöèîíàëüíóþ ôàçó: 21.07.2004 (74) Ïàòåíòíûé ïîâåðåííûé: Åãîðîâà Ãàëèíà Áîðèñîâíà (86) Çà âêà PCT: FR 02/04344 (13.12.2002) Àäðåñ äë ïåðåïèñêè: 129010, Ìîñêâà, óë. Á.Ñïàññêà , 25, ñòð.3, ÎÎÎ "Þðèäè÷åñêà ôèðìà Ãîðîäèññêèé è Ïàðòíåðû", ïàò.ïîâ. Ã.Á. Åãîðîâîé R U Ôîðìóëà èçîáðåòåíè 1. Ñïîñîá ïîëó÷åíè ëàêòàìà âçàèìîäåéñòâèåì ñîåäèíåíè , âûáðàííîãî èç ãðóïïû, ñîäåðæàùåé ñëîæíûå ýôèðû èëè àìèäû 6-àìèíîêàïðîíîâîé êèñëîòû, èëè èõ ñìåñè, îòëè÷àþùèéñ òåì, ÷òî âçàèìîäåéñòâèå îñóùåñòâë þò â ïàðîâîé ôàçå è â ïðèñóòñòâèè òâåðäîãî êàòàëèçàòîðà. 2. Ñïîñîá ïî ï.1, îòëè÷àþùèéñ òåì, ÷òî òâåðäûé êàòàëèçàòîð âûáèðàþò èç ãðóïïû, ñîäåðæàùåé îêñèäû ìåòàëëîâ, öåîëèòû, ãëèíû, ôîñôàòû ìåòàëëîâ. 3. Ñïîñîá ïî ï.2, îòëè÷àþùèéñ òåì, ÷òî ãëèíó âûáèðàþò èç êàîëèíîâ, ñåðïåíòèíîâ, ñìåêòèòîâ èëè ìîíòìîðèëëîíèòîâ, èëëèòîâ èëè ñëþä, ãëàóêîíèòîâ, õëîðèòîâ èëè âåðìèêóëèòîâ, àòòàïóëüãèòîâ èëè ñåïèîëèòîâ, ñìåøàííîñëîéíûõ ãëèí, àëëîôàíîâ èëè èìîãîëèòîâ è ãëèí ñ âûñîêèì ñîäåðæàíèåì îêñèäà àëþìèíè . 4. Ñïîñîá ïî ï.3, îòëè÷àþùèéñ òåì, ÷òî ãëèíà ïðåäñòàâë åò ñîáîé ìîíòìîðèëëîíèò. 5. Ñïîñîá ïî ëþáîìó èç ï.3 èëè 4, îòëè÷àþùèéñ òåì, ÷òî ãëèíà âë åòñ ãëèíîé ñ ìîñòèêîâûìè ñâ ç ìè. 6. Ñïîñîá ïî ï.1 èëè 2, îòëè÷àþùèéñ òåì, ÷òî êàòàëèçàòîð ïðåäñòàâë åò ñîáîé ñîñòî ùèé èç ÷àñòèö êàòàëèçàòîð, ïîëó÷åííûé ôîðìîâàíèåì, ïî ìåíüøåé ìåðå, îäíîãî ïðîñòîãî èëè ñìåøàííîãî íåîðãàíè÷åñêîãî îêñèäà, ïî ìåíüøåé ìåðå, îäíîãî ýëåìåíòà, âûáðàííîãî èç ãðóïïû, ñîñòî ùåé èç êðåìíè , àëþìèíè , òèòàíà, öèðêîíè , âàíàäè , íèîáè , òàíòàëà, âîëüôðàìà, ìîëèáäåíà, æåëåçà, ðåäêîçåìåëüíûõ ýëåìåíòîâ è îí ñîäåðæèò, ïî ìåíüøåé ìåðå, îäíó ìàêðîïîðèñòîñòü, ...

N- (a-acyloxyethyl) compound and preparation method thereof

비교적 온화한 조건하에서 열분해반응에 의해 산업적으로 매우 중요한 N-비닐 화합물, 즉 N-비닐-2-피롤리돈으로 전환할 수 있고 신규한 화합물인 N-( -아실옥시에틸)-화합물, 즉 N-( -아실옥시에틸)-2-피롤리돈 및 N-( -아실옥시에틸)-화합물의 제조방법이 제안되어 있다. N-(

Quaternary substituted bleach activators

Bleaching compositions, laundry and automatic dishwashing detergent compositions comprising particular quaternary-substituted bleach activators, are provided. More specifically, the invention relates to compositions which provide enhanced cleaning/bleaching benefits though the selection of quaternary-substituted bleach activators having specific leaving groups with a conjugate acid pKa above 13 and with specific ratios of the rate of perhydrolysis to the rate of hydrolysis and the rate of perhydrolysis to the rate of diacylperoxide production. Included are preferred activator compounds and methods for washing fabrics, hard surfaces, and tableware using the activators.

Method for preparing 4R-hydroxy-N-benzyl-2-piperidinone

본 발명은 고지혈증 치료제인 아토르바스타틴을 제조하기 위한 핵심 중간체인, 4R-하이드록시-N-벤질-2-피페리디논의 제조방법에 관한 것으로, 2,4-디옥소-N-벤질-피페리딘을 루테늄 촉매하에서 고압 수소화 반응시키는 것을 포함하는 본 발명의 방법에 의하면, 4R-하이드록시-N-벤질-2-피페리디논을 종래의 방법에 비해 온화한 조건하에서 간편하게 고수율로 합성할 수 있다.

Solid composition consisting of heterocyclic compounds and/or oxime esters and inert porous carrier materials and the use thereof as stable bleach activator component in detergents, bleaches and cleaners

A solid composition consisting essentially of 5-98 parts by weight of heterocyclic compounds I where L 1 is groups with a cyclic carbamate, a lactonoxy or a lactam structure, X is a carbonyl, a doubled carbonyl or a heterocarbonyl group, and R 1 is an organic radical or a second moiety L 1 , and/or oxime esters II where L 2 is an oxime moiety where R 2 , R 3 and Z 4 are organic radicals or linkers, L 3 is the radical R 1 , a second oxime moiety L 2 or a carboxylic ester residue, carboxamide residue, phenolate residue, vinyloxy radical, sulfonamide residue, imidazole residue, amidolactam residue, cyclic carbamate residue, lactonoxy residue or lactam residue, and m is 0 or 1, and 2-95 parts by weight of inert porous carrier materials with an internal surface area of from 10 to 500 m 2 /g. The solid composition described is suitable as stable bleach activator component in detergents, bleaches and cleaners.

Bleaching compositions comprising n-acyl caprolactam activators

Bleaching compounds comprising substituted benzoyl caprolactam bleach activators

Laundry detergents and bleaching systems which comprise substituted benzoyl caprolactam bleach activators are presented having the formula: wherein R1, R2, R3, R4, and R5 are members selected from the group consisting of H, halogen, alkyl, alkoxy, alkoxyaryl, alkaryl, alkaryloxy, NO2, and members having the structure: wherein R6 is selected from the group consisting of H, alkyl, alkaryl, alkoxy, alkoxyaryl, alkaryloxy, and aminoalkyl; X is O, NH, or NR7, wherein R7 is H or a C1-C4 alkyl group; and R8 is an alkyl, cycloalkyl, or aryl group containing from 3 to 11 carbon atoms; provided that at least one R substituent is not H. The bleach activators are effective under mixed soil conditions, especially mixtures of hydrophobic and hydrophilic soils and stains.

Acyl valerolactam bleach activators

Quarternary substituted bleach activators

Bleaching compositions, laundry and automatic dishwashing detergent compositions comprising particular quaternary-substituted bleach activators, are provided. More specifically, the invention relates to compositions which provide enhanced cleaning/bleaching benefits though the selection of quaternary-substituted bleach activators having specific leaving groups with a conjugate acid pKa above 13 and with specific ratios of the rate of perhydrolysis to the rate of hydrolysis and the rate of perhydrolysis to the rate of diacylperoxide production. Included are preferred activator compound s and methods for washing fabrics, hard surfaces, and tableware using the activators.

1,3-disubstituted (2-thio)'ureas having effect on mnestic processes

A 1,3-disubstituted urea or 2-thiourea having the formula <IMAGE> wherein R1, R2, R3, R6, R7 and R8 represent independently a hydrogen atom, an alkyl radical containing 1 to 4 carbon atoms, an alkenyl radical containing 2 to 4 carbon atoms, an alkylene radical forming together with the carbon atom to which it is attached a cycloalkane ring having 5 or 6 carbon atoms, an aryl radical or a substituted aryl radical, R4 and R5 represent independently a hydrogen atom, an alkyl radical containing 1 or 2 carbon atoms or a phenyl radical, n and q are independently a whole number of from 3 to 7, m and p are independently 0, 1 or 2 and X is an oxygen or a sulfur atom, processes for the preparation thereof and pharmaceutical compositions containing the same.

Substitute hydroxyphenyl-piperidones

Piperidine derivatives - as uv and heat stabilizers for polymers

Title derivs of formula: (in which A is -CH2-, -CH2CH2- or -CH-CH2-; R1 and R2 are straight or branched chain alkyl radicals, pref. R2 is t-butyl ortho to the -OH or -cH3, ortho or meta to the OH, n is 0 or 1) or their salts with acid are used as stabilisers of polymers, partic high or low density polyethylene, polypropylene or polystyrene, against UV light, oxidation and heat, without altering the colour.

Process for the production of omega-omega'-diaminoalkanes

O-methyl lactime ethers prepn - from lactam and dimethyl sulphate and treatment with a strong inorganic base

Title cpds. having 6-9 ring atoms are prepd. by reacting lactam having 6-9 ring atoms with at least an equimolecular quantity of dimethylsulphate and treating the product with at least an equivalent amount (based on the dimethylsulphate initially used) of an aq. soln. of a strong inorganic base at 25-100 degrees C (pref. 30-70 degrees C) opt. in the presence of a non- or only slightly water miscible inert solvent, so that the free O-methyl lactime ether contains at most only traces of dimethylsulphate. The products are inters for N-methyllactams, pharmaceuticals, perfumes, fungicides, algicides, bactericides. etc.

Process for preparing alpha-amino-epsilon-caprolactam

Patent FR2277585B1

Oxime carbamate cpds - with pesticidal activity

Carbamates of formula (I): (where A is tetra- or pentamethylene opt. substituted by 1-4C alkyl; R1 is alkyl or (opt. substituted) cycloalkyl, aralkyl or phenyl and R2 is 1-4C alkyl, or NR1R2 is a saturated heterocyclic residue; and R3 is alkyl, alkenyl, alkynyl, cyclohexyl or benzyl). Insecticides, acaricides and nematocides with marked systemic activity, favourable toxicity towards warm-blooded animals and a lack of phytotoxicity. Suitable for use in plant-protection, protecting stored goods and soil-treatment.

Process for the production of aromatic aminosulfonylamidines

(2-THIO) 1,3-DISUBSTITUTED UREES FOR USE AS MEDICINAL PRODUCTS

a. Urées et thiourées 1,3-disubstituées. b. (2-Thio)urées 1,3-disubstituées répondant à la formule générale : at. 1,3-disubstituted ureas and thioureas. b. 1,3-disubstituted (2-Thio) ureas corresponding to the general formula:

N-alkyllactams prodn

N-alkyllactams (1-4C alkyl) are made by treating the corresponding unsubtsd. lactam (4-8C in the ring) with a sym. dialkyl ether (about 2-fold excess) with a water-splitting catalyst (esp. Al2O3) at 250-350 degrees C. Yields are around 65-75%.

PROCESS FOR THE PREPARATION OF N, N'-CARBONYLBISLACTAMES

Patent FR2380262B1

Lysine synthesis process

Antihypertonic lactam oxime-carbamates - prepd by reacting lactam oximes with carbamoyl halides

Lactamoximcarbamates are of formula (I): (where n = 3-7; and R1 and R2 are H or 1-3C alkyl). Cpd. is pref. (I: n = 6; R1 H; R2 = methyl), tautomers and salts. (I) have circulatory activity with low toxicity and are pref. used in the treatment of hypertonie.

Patent FR8129M

New amino-azacycloheptanones, their preparation and applications

Method for pilot-plant-scale production of caprolactam in micro-reaction device

本发明公开了一种微反应装置中试放大生产己内酰胺的方法，它是一种以环己酮肟和三氟乙酸为原料，利用微反应装置高效生产己内酰胺的方法。与现有技术相比，本发明工艺简单，能耗较低，具有较高的操作安全性；同时，本发明转化率及终产物选择性都极高，是一种绿色环保高效的合成己内酰胺的方法，为工业化放大生产提供重要数据参考。

ACID HALOGENIDE AND / OR ACYLLACTAM FUNCTIONAL COMPOUNDS AND POLYLACTAM BLOCK COPOLYMERS DERIVED THEREFROM.

Purification of N-vinyl-ε-caprolactam

A process for purifying N-vinyl-ε-caprolactam comprises converting the N-vinyl-ε-caprolactam which is to be purified and has a purity of at least 95% by weight into a melt, partially crystallizing the melt and separating the crystals from the mother liquor.

HYDROXYPHENYL-PIPERIDONES SUBSTITUTES, THEIR PREPARATION PROCESS AND THEIR APPLICATION

A kind of method utilizing microreactor to be prepared caprolactam by alpha-amido-epsilon-caprolactams

本发明公开了一种利用微反应器由α‑氨基‑ε‑己内酰胺制备己内酰胺的方法，将α‑氨基‑ε‑己内酰胺和氢氧化钾溶解在水中，得溶液a，再将羟胺‑O‑磺酸溶解在水中，得溶液b，将溶液a和溶液b同时分别泵入微通道模块化反应装置，在低温微结构反应器中，‑5～5℃、pH 8～12条件下停留2～15min，低温微结构反应器出料再通入高温微结构反应器中，在90～100℃条件下停留2～15min，将反应产物浓缩后导入分离装置，加入有机溶剂进行萃取，得到有机萃取液合并，减压蒸馏除溶剂，得到最终的产物己内酰胺。本发明方法制备工艺易操作控制，具有工业放大潜力。

Preparation process for n,n'-carbonylbis-lactams

L'invention concerne un procédé de préparation des N,N'-carbonylbislactames par réaction du phosgène avec au moins un lactame qui est caractérisé en ce que l'amine tertiaire est choisie dans le groupe constitué par les amines tertiaires aliphatiques non nucléophiles. On obtient ainsi des N,N'-carbonylbislactames de pureté élevée et avec de bons rendements aussi bien au laboratoire qu'à l'échelon industriel.

7-Phenyl-quinolizidine derivatives (I), their preparation, pharmaceutical compositions containing them and (I) for use in treating diseases.

Phenyl-quinolizidines of the formula < IMAGE > I wherein X, Y, R1 and R2 are as hereinafter set forth, are described. The compounds of formula I are useful as antipsychotics, antiemetics and analgesics.

Patent FR2227001A1

SUBSTITUTED HYDROXYPHENYL PIPERIDONES

PROCESS FOR THE PREPARATION OF (2-THIO) -1,3-DISUBSTITUTED UREASES

Lactam synthesizing method

A method of continuously manufacturing lactam under high temperature and high pressure fluid, characterized by comprising the step of leading ketone and a hydroxylamine compound in a reaction field under high temperature and high pressure conditions of circulating fluid to efficiently synthesize lactam in a short time, whereby lactam can be rapidly synthesized continuously from ketone under the high temperature and high pressure fluid conditions of 175°C or higher in temperature range and 7 MPa or higher in pressure range.

NOVEL DERIVATIVES OF VARIOUSLY SUBSTITUTED CYCLIC AMIDES SELECTIVE ANTAGONISTS OF THE HUMAN NK3 RECEPTOR, PROCESS FOR THEIR PRODUCTION AND PHARMACEUTICAL COMPOSITIONS CONTAINING THEM

Preparation of lactams

Curable powder coating compositions containing caprolactam-blocked isocyanates

A curable powder coating composition comprising: (i) TMXDI/e-caprolactam adduct and (ii) isoayanate reactive material such as hydroxy-functional acrylic resin of polyester is described. The preparation of TMXDI-e-caprolactam blocked iscoyanate is also described.

Patent FR2106145A5

Conveyor chain for container nest

This relates to a special endless conveyor chain particularly adapted to carry fixtures which are to be readily removable and replaceable on the conveyor chain. In order to accomplish this, the pins which connect together the links of a conventional conveyor chain are elongated above the conveyor chain for reception in bores within an associated fixture. The conveyor chain is formed of elongated links and shorter links with the length of the elongated links being in accordance with the general dimensions of a fixture longitudinally of the conveyor chain. Each upper one of the elongated links is provided with a flat upper surface so as to provide a supporting surface for a fixture to be mounted thereon. Instead of the usual strap-like configuration, each upper elongated link is preferably provided with an enlarged central portion which may be circular in outline to provide an adequate seat for an associated fixture. A special sprocket may be provided for the conveyor chain with the sprocket having circumferentially spaced teeth for reception between customary rollers of the conveyor chain and with the sprocket further having between each pair of teeth a radially outwardly projection for projecting between elongated links of the conveyor chain with the sprocket projection being in supporting relation with respect to an associated upper elongated link whereby a loading placed on a fixture carried by the conveyor chain is first transmitted to an associated upper elongated link and through that link to the underlying sprocket projection.

Process for the preparation of monoblocked (cyclo) aliphatic diisocyanates

Process for preparing d, l-alpha-amino-caprolactam

Novel actibator for synthesizing polyamide and polyamide prepared therefrom

신규한 폴리아미드 합성용 활성화제 및 그로부터 제조된 폴리아미드가 제공된다. Novel activators for polyamide synthesis and polyamides prepared therefrom are provided.

Phenyl-quinolizidines their manufacture and pharmaceutical compositions containing them

5-thio-piperdinyl prostaglandin e analogs

A compound comprising (I) or a pharmaceutically acceptable salt or a prodrug thereof is disclosed herein. Y and R are described in detail herein. A compound having an .omega. chain comprising (II) or a derivative thereof, or a pharmaceutically acceptable salt or a prodrug thereof, is disclosed. Derivatives, salts and prodrugs are identified and described in detail. Methods of treating certain conditions or diseases, and compositions and medicaments related thereto are also contemplated.

METHOD OF OBTAINING CAPROLACTAM

Получение капролактама путем превращения 6-аминокапронитрила с водой в присутствии катализаторов, заключающееся в том, что используют исходную смесь из аминокапронитрила и тетрагидроазепинпроизводного, имеющего формулу (1), и превращение проводят в жидкой фазе в присутствии гетерогенных катализаторов, а также способ получения тетрагидроазепинпроизводного (1) и его применение для получения капролактама и поликапролактама.Международная заявка была опубликована вместе с отчетом о международном поиске. Obtaining caprolactam by converting 6-aminocapronitrile with water in the presence of catalysts, which consists in using an initial mixture of aminocapronitrile and tetrahydroazepine derivative having formula (1), and the conversion is carried out in the liquid phase in the presence of heterogeneous catalysts, and also a method of producing a tetrahydroazepine derivative (1 ) and its use for caprolactam and polycaprolactam. The international application was published together with an international search report.

Lactam-n-carboxylic acid chlorides and their production

THE PRODUCTION OF LACTAM-N-CARBOXYLIC ACID CHLORIDES HAVING 5 TO 13 RING MEMBERS BY REACTING WITH A HYDROGEN HALIDE A 1-AZA-2-HYDROXYCYCLOALKENE-(2)-CARBOXYLIC ACID CHLORIDE-(1) WHICH IS ETHERIFIED IN THE 2-POSTION. LACTAMN-CARBOXYLIC ACID CHLORIDES ARE SUITABLE FOR THE PRODUCTION OF N-SUBSTITUTED LACTAMS FROM WHICH THE CORRESPONDINGLY SUBSTITUTED POLYAMIDES MAY BE PRODUCED.

Patent JPS6241220B2