公开(公告)号：WO02102772B1

公开(公告)日：2003-11-20

申请号：PCT/US0219372

申请日：2002-06-17

Applicant: BATTELLE MEMORIAL INSTITUTE

Inventor： WERPY TODD ,  FRYE JOHN G JR ,  WANG YONG ,  ZACHER ALAN H

IPC: C07D207/26 ,  C07D207/267

CPC classification number: C07D207/267 ,  C07D201/02 ,  C07D201/08

Abstract: The present invention provides methods for making N-methylpyrrolidine and analogous compounds via hydrogenation. Novel catalysts for this process, and novel conditions/yields are also described. Other process improvements may include extraction and hydrolysis steps. Some preferred reactions take place in the aqueous phase. Starting materials for making N-methylpyrrolidine may include succinic acid, N-methylsuccinimide, and their analogs.

Abstract translation: 本发明提供了通过氢化制备N-甲基吡咯烷和类似化合物的方法。 还描述了用于该方法的新型催化剂和新的条件/收率。 其他工艺改进可以包括提取和水解步骤。 一些优选的反应发生在水相中。 用于制备N-甲基吡咯烷的原料可包括琥珀酸，N-甲基琥珀酰亚胺及其类似物。

公开(公告)号：WO0228525A9

公开(公告)日：2002-11-28

申请号：PCT/NL0100728

申请日：2001-10-03

Applicant: DSM NV ,  GUIT RUDOLF PHILIPPUS MARIA ,  NOTTEN MATHIEU JOHANNES GUILLA ,  PESTMAN ROBERT

Inventor： GUIT RUDOLF PHILIPPUS MARIA ,  NOTTEN MATHIEU JOHANNES GUILLA ,  PESTMAN ROBERT

IPC: B01J19/02 ,  B01J19/24 ,  B01J23/46 ,  C07D201/08

CPC classification number: B01J19/02 ,  B01J23/462 ,  B01J2219/0236 ,  B01J2219/0277 ,  B01J2219/0286 ,  C07D201/08

Abstract: Process for the preparation of a mixture of epsilon -caprolactam and epsilon -caprolactam precursors by reductively aminating 5-formylvaleric acid and/or 5-formylvalerate ester(s) in water with hydrogen and an excess of ammonia in the presence of a hydrogenation catalyst, wherein the process is conducted in a reactor of which the inside reactor wall material is a material containing at most 8 wt.% nickel.

Abstract translation: 通过在氢化催化剂存在下，用氢气和过量的氨将水中的5-甲酰戊酸和/或5-甲酰戊酸酯还原胺化制备ε-己内酰胺和ε-己内酰胺前体的混合物的方法， 其中所述方法在其内反应器壁材料是含有至多8重量％镍的材料的反应器中进行。

公开(公告)号：WO01096294A1

公开(公告)日：2001-12-20

申请号：PCT/EP2001/006687

申请日：2001-06-13

IPC: C07D233/10 ,  C07B61/00 ,  C07D201/08 ,  C07D223/10

CPC classification number: C07D201/08 ,  Y02P20/52

Abstract: The invention relates to a method for the production of caprolactam from a compound of formula (I): NC-(CH2)5-CO-R where R = a carboxamido, carboxlic acid or carboxylate ester group, characterised in that a) a compound (I), or mixtures thereof are hydrogenated with hydrogen in the presence of ammonia, a catalyst (II) and optionally a fluid solvent (VI) to give a mixture (III), b) separation of catalyst (II) and hydrogen from the mixture (III) to give a mixture (IV) and c) reaction of mixture (IV), in the presence of a catalyst (V) and optionally a fluid solvent (VII), to give caprolactam.

Abstract translation: NC-（CH2）5-CO-R，其中R：羧酸酰胺，羧酸或其特征在于羧酸酯基）的化合物（I）或它们的混合物，一种从式（I）的化合物的制备己内酰胺的方法 如果合适的液体稀释剂（VI）在催化剂（II）的存在下氢氨和存在下进行氢化，得到的混合物（III），b）从所述混合物（III）为氢和催化剂（II）被分离，得到的混合物（IV） 和c）将混合物（IV）任选的（在液体稀释剂VII的在催化剂（V）的存在下存在）的反应，己内酰胺。

公开(公告)号：WO01083443A1

公开(公告)日：2001-11-08

申请号：PCT/EP2001/004837

申请日：2001-04-30

IPC: C07D223/12 ,  C07D201/08

CPC classification number: C07D201/08

Abstract: The invention relates to a method for producing caprolactam, which is characterized by a) reacting, in the presence of a catalyst, a mixture (I) that contains 6-aminocapronitrile and water in the gaseous phase to give a mixture (II) that contains caprolactam, ammonia, water, high-boiling and low-boiling substances, subsequently b) removing the ammonia from mixture (II), thereby producing a mixture (III) that contains caprolactam, water, high-boiling and low-boiling substances, c) removing the water from mixture (III), thereby producing a mixture (IV) that contains caprolactam, high-boiling and low-boiling substances, and finally d) obtaining by crystallization a caprolactam-containing solid substance (V) from mixture (IV), the weight percentage of caprolactam in the solid substance (V) being higher than in mixture (IV).

Abstract translation: 一种用于含有己内酰胺，氨，水，高沸点和低沸点在催化剂的存在下，然后将包含在气相中（共混物II）6-氨基己腈与水在制备己内酰胺，其特征在于，a）的混合物（I）的过程 b）从所述混合物（II）的氨除去，得到含有己内酰胺，高沸点和低沸点的混合物（III），其包括从（III）的水被除去，混合物己内酰胺，水，高沸点和低沸点，然后c）（以得到的混合物IV），和 然后d）为从混合物（IV）由结晶化的含有己内酰胺的固体（V），其特征在于，按重量计在固体（V己内酰胺的比例）比在混合物（IV）大。

公开(公告)号：WO9951568A3

公开(公告)日：1999-11-18

申请号：PCT/US9906822

申请日：1999-03-29

Applicant: DU PONT PHARM CO

Inventor： ZHOU JICHENG ,  OH LYNETTE MAY ,  MA PHILIP

IPC: C07D261/08 ,  C07B61/00 ,  C07C253/00 ,  C07C255/17 ,  C07C255/40 ,  C07D201/08

CPC classification number: C07C253/00 ,  C07D201/08 ,  C07C255/17 ,  C07C255/40

Abstract: The present invention relates to processes for the production of alpha -aryl- beta -ketonitriles, which serve as synthetic intermediates in the preparation of a series of biologically important molecules such as corticotropin releasing factor (CRF) receptor antagonists.

Abstract translation: 本发明涉及制备α-芳基-β-酮腈的方法，其用作制备一系列重要生物学分子如促肾上腺皮质激素释放因子（CRF）受体拮抗剂的合成中间体。

公开(公告)号：WO99048867A1

公开(公告)日：1999-09-30

申请号：PCT/NL1999/000148

申请日：1999-03-17

IPC: C07D201/08 ,  C07D201/16

CPC classification number: C07D201/08 ,  C07D201/16

Abstract: The invention relates to a process for the purification of crude epsilon -caprolactam, wherein crude epsilon -caprolactam prepared by cyclization of alkyl 6-aminocaproate, 6-aminocapronitrile, 6-aminocaproic acid, 6 aminocaproic amide and/or oligomers thereof, is subjected to a crystallization process.

Abstract translation: 本发明涉及一种纯化ε-己内酰胺的方法，其中将通过6-氨基己酸烷基酯，6-氨基己腈，6-氨基己酸，6-氨基己酰胺和/或其低聚物的环化制备的粗ε-己内酰胺进行 结晶过程。

公开(公告)号：WO98037063A1

公开(公告)日：1998-08-27

申请号：PCT/NL1998/000082

申请日：1998-02-10

IPC: C07D201/08

CPC classification number: C07D201/08

Abstract: Process to prepare epsilon -caprolactam by treating 6-aminocaproic acid, 6-aminocaproate ester or 6-aminocaproamide or mixtures comprising at least two of these compounds in the presence of superheated steam in which a gaseous mixture comprising epsilon -caprolactam and steam is obtained, wherein the process is carried out in the absence of a catalysts at a temperature between 250 and 400 DEG C and at a pressure of between 0.5 and 2 MPa. The invention also encompasses a process to prepare epsilon -caprolactam starting from 6-aminocapronitrile by performing a hydrolysis and a subsequent step as described above.

Abstract translation: 在过热蒸汽的存在下，通过在其中得到包含ε-己内酰胺和蒸汽的气体混合物的情况下，通过处理6-氨基己酸，6-氨基己酸酯或6-氨基己酰胺或包含这些化合物中至少两种的混合物来制备ε-己内酰胺的方法， 其中所述方法在不存在催化剂的情况下在250-400℃和0.5-2MPa的压力下进行。 本发明还包括通过进行如上所述的水解和后续步骤从6-氨基己腈开始制备ε-己内酰胺的方法。

公开(公告)号：WO1998017642A1

公开(公告)日：1998-04-30

申请号：PCT/NL1997000467

申请日：1997-08-14

Applicant: DSM N.V. ,  E.I. DU PONT DE NEMOURS AND COMPANY ,  GUIT, Rudolf, Philippus, Maria

Inventor： DSM N.V. ,  E.I. DU PONT DE NEMOURS AND COMPANY

IPC: C07D201/16

CPC classification number: C07D201/16 ,  C07D201/08

Abstract: Process to separate epsilon -caprolactam from 6-aminocaproamide and 6-aminocaproamide oligomers, wherein epsilon -caprolactam, 6-aminocaproamide and 6-aminocaproamide oligomers are present in a first aqueous starting mixture, which mixture is contacted with an alcohol extraction solvent, resulting in a first aqueous raffinate phase which is poor in epsilon -caprolactam and an alcohol phase which is rich in epsilon -caprolactam and which alcohol phase contains 6-aminocaproamide and/or 6-aminocaproamide oligomers, wherein the latter alcohol phase is subsequently contacted with water (backwash water) resulting in an alcohol extract phase poor in 6-aminocaproamide and/or 6-aminocaproamide oligomers and a second aqueous raffinate phase rich in 6-aminocaproamide and/or 6-aminocaproamide oligomers.

Abstract translation: 将ε-己内酰胺与6-氨基己酰胺和6-氨基己酰胺低聚物分开的方法，其中ε-己内酰胺，6-氨基己酰胺和6-氨基己酰胺低聚物存在于第一含水起始混合物中，该混合物与醇提取溶剂接触，导致 ε-己内酰胺差的第一含水萃余液相和富含ε-己内酰胺的醇相，其中醇相含有6-氨基己酰胺和/或6-氨基己酰胺低聚物，其中后一个醇相随后与水接触（ 反洗水）导致6-氨基己酰胺和/或6-氨基己酰胺低聚物中的醇提取相差和富含6-氨基己酰胺和/或6-氨基己酰胺低聚物的第二含水萃余液相。

公开(公告)号：WO1996017826A1

公开(公告)日：1996-06-13

申请号：PCT/EP1995004680

申请日：1995-11-29

Applicant: BASF AKTIENGESELLSCHAFT

Inventor： BASF AKTIENGESELLSCHAFT ,  FUCHS, Eberhard ,  ACHHAMMER, Günther

IPC: C07D201/08

CPC classification number: C07D201/08 ,  Y02P20/52 ,  Y10S203/17 ,  Y10S203/90

Abstract: Method for preparing caprolactam by heating 6-aminocapric acid nitrile in the presence of heterogeneous catalysts ans water under elevated pressure, wherein (a) 6-aminocapric acid nitrile or a mixture containing essentially 6-aminocapric acid nitrile as well as water and a low-boiling or a high-boiling alcohol is heated in the presence of a heterogeneous catalyst in a reactor A to produce a mixture (I); then (b) mixture (I) is distilled, yielding a head fraction, caprolactam and a bottom product, with any ammonia in mixture (I) being removed prior to distillation; and then (c1) the head fraction is fed into the reactor of step (a), with the head fraction optionally being mixed with the alcohol and/or water and/or 6-aminocapric nitrile used in step (a) before being fed into reactor (A); or (c2) the head fraction, optionally with the bottom product from step (b), is fed into a reactor (B), the first fraction optionally being mixed with the alcohol and/or water and/or 6-aminocapric acid nitrile before being fed into reactor (B), and then analogously to step (b) caprolactam is produced by distillation; and either (d1) the bottom product from step (b) is fed into reactor A of step (a); or (d2) optionally water and possibly a low-boiling or a high-boiling alcohol are added to the bottom product which then, analogously to step (a) is heated in a reactor (C) to give a reaction product which is distilled to yield caprolactam; or (d3) water is added to the bottom product which is heated in a reactor (D) without added catalyst to give a reaction product which is distilled to yield caprolactam; or (d4) water and a base are added to the bottom product which is heated in reactor (E) to give a reaction product which is distilled to yield caprolactam.

Abstract translation: 己内酰胺通过加热在升高的压力6-氨基己腈在非均相催化剂的存在下，和水，通过使制备（a）6-氨基己腈或基本上含6-氨基己腈，和水和光，或在高沸点醇的混合物 在反应器（a）中的非均相催化剂的存在下加热，得到的混合物（I）; 然后（b）的混合物（I）进行蒸馏，得到顶部馏分，己内酰胺和底部，其中，一个，如果混合物（I）的氨，在此之前蒸馏除去，然后（C1）的顶部馏分到反应器（A） 步骤（a）如果需要的话在步骤设置馈送得到醇Kopfraktion（a）和/或水和/或6-氨基己腈被送入反应器（A）之前进行混合; 或（C2）的顶部馏分，如果需要的话，与来自阶段底部产物（b）中引入反应器（B），得到醇的顶部馏分送入，如果需要设置在步骤（a）和/或水和/或6-氨基己腈前 供给到反应器（b）混合，然后同样地阶段（b）回收通过蒸馏己内酰胺; 并且或者（D1）从步骤步骤（b）（A）的底部产物（a）进料到反应器中; 或（D2）的底部任选地与水混合，并且如果需要的话，具有光或高沸点醇，然后在类似于步骤（a）中加热，得到反应后的混合物进一步反应器（C），和己内酰胺通过蒸馏从得到的反应产物中回收 ; 或（D3）中的溶液与水和不添加在加热得到反应后的混合物的反应器（D）的催化剂的贮槽，和己内酰胺通过蒸馏从得到的反应产物中回收; 或（D4）与水和在加热得到反应后的混合物的反应器（E）的基贮槽和己内酰胺通过蒸馏从得到的反应产物中回收的混合。

公开(公告)号：WO1995014665A1

公开(公告)日：1995-06-01

申请号：PCT/EP1994003782

申请日：1994-11-15

Applicant: BASF AKTIENGESELLSCHAFT ,  FUCHS, Eberhard ,  WITZEL, Tom

Inventor： BASF AKTIENGESELLSCHAFT

IPC: C07D201/08

CPC classification number: C07D201/08

Abstract: A process is proposed for the production of cyclic lactams by allowing aminocarboxylic acid nitriles to react with water in the presence of catalysts. The reaction takes place in the fluid phase in a fixed bed reactor in the presence of heterogeneous catalysts, no constituents of which are soluble under these reaction conditions.

Abstract translation: 通过在催化剂存在下，其中，在具有在反应条件下不溶性成分的非均相催化剂的存在下，固定床反应器，该反应是在液相中进行氨基腈与水反应而制备的环状内酰胺。