公开(公告)号：US06479658B1

公开(公告)日：2002-11-12

申请号：US09744210

申请日：2001-06-04

Applicant: Jean-Pierre Brunelle ,  Aline Seigneurin ,  Lionel Sever

Inventor： Jean-Pierre Brunelle ,  Aline Seigneurin ,  Lionel Sever

IPC: C07D22308

CPC classification number: C07D201/08

Abstract: The invention relates to a process for the cyclizing hydrolysis of an aminonitrile compound into a lactam in the presence of a catalyst. The invention relates more particularly to a process for the cyclizing hydrolysis of an aminonitrile compound in the presence of a macroporous particulate catalyst obtained by deposition/impregnation of an oxygenated compound onto a macroporous support such as alumina. The invention applies in particular to the preparation of &egr;-caprolactam by cyclizing hydrolysis of aminocapronitrile.

Abstract translation: 本发明涉及一种在催化剂存在下使氨基腈化合物环化成内酰胺的方法。本发明涉及一种在大孔颗粒催化剂存在下环化氨基腈化合物的水解方法，该方法由 将氧合化合物沉积/浸渍到大孔载体如氧化铝上。 本发明特别适用于通过环化氨基己腈的水解制备ε-己内酰胺。

公开(公告)号：US06362333B1

公开(公告)日：2002-03-26

申请号：US09786940

申请日：2001-03-12

Applicant: Martin Merger ,  Rolf Fischer ,  Andreas Ansmann

Inventor： Martin Merger ,  Rolf Fischer ,  Andreas Ansmann

IPC: C07D20108

CPC classification number: C07D201/02 ,  C07D201/08 ,  C07D295/023

Abstract: A cyclic lactam and a cyclic amine are coproduced by coreacting an aliphatic alpha, omega-diamine and an aliphatic alpha, omega-aminonitrile with water in the gas phase in the presence of a heterogeneous catalyst.

Abstract translation: 通过在非均相催化剂的存在下，在气相中与脂肪族α，ω-二胺和脂族α，ω-氨基腈与水共核反应来共同制备环状内酰胺和环胺。

公开(公告)号：US06353100B1

公开(公告)日：2002-03-05

申请号：US09260143

申请日：1999-03-01

Applicant: Rudolf P. M. Guit ,  Wim Buijs

Inventor： Rudolf P. M. Guit ,  Wim Buijs

IPC: C07D20100

CPC classification number: C07D201/08

Abstract: Process for the preparation of &egr;-caprolactam, in which in a step (a) a compound with the general formula: O=CH—(CH2)4—C(O)—R  (1) in which R is —OH, —NH2 or O—R′, in which R′ is an organic group with 1 to 10 carbon atoms, is contacted with ammonia and hydrogen in a suitable solvent at elevated pressure in the presence of a hydrogenation catalyst to a mixture of primary amino compounds and &egr;-caprolactam, followed by a separate second step (b) in which the primary amino compounds are reacted to &egr;-caprolactam, wherein the solvent in step (a) is an aqueous medium, including water, the yield to &egr;-caprolactam in step (a) is more than 10%, calculated on the initial molar amount of the compound according to formula (1), that &egr;-caprolactam is separated from the aqueous mixture obtained in step (a) by extraction and that the aqueous mixture resulting from the extraction, containing the primary amino compounds, is used in step (b).

Abstract translation: 制备ε-己内酰胺的方法，其中在步骤（a）具有以下通式的化合物：其中R是-OH，-NH 2或O-R'，其中R'是有机基团，其中1至 10的碳原子在合适的溶剂中，在氢化催化剂的存在下，在氨基酸和ε-己内酰胺的混合物中，在合适的溶剂中与氨和氢接触，随后分开第二步（b），其中伯氨基 化合物与ε-己内酰胺反应，其中步骤（a）中的溶剂是水性介质，包括水，步骤（a）中ε-己内酰胺的收率大于10％，根据化合物的初始摩尔量计算 根据式（1），通过萃取将ε-己内酰胺与步骤（a）中获得的含水混合物分离，并且在步骤（b）中使用含有伯氨基化合物的萃取产生的含水混合物。

公开(公告)号：US06222033B1

公开(公告)日：2001-04-24

申请号：US09403655

申请日：1999-10-25

Applicant: Eberhard Fuchs ,  Rolf Fischer

Inventor： Eberhard Fuchs ,  Rolf Fischer

IPC: C07D20108

CPC classification number: C07D201/08

Abstract: The disclosure is a process for preparing cyclic lactams of the formula I: where R1 is hydrogen, alkyl, cycloalkyl or aryl, and A is C3-C12-alkylene unsubstituted or substituted by 1, 2, 3, 4, 5 or 6 substituents selected independently of one another from the group consisting of alkyl, cycloalkyl and aryl, by conversion of an &ohgr;-aminocarbonitrile of the formula II: HR1N—A—CN  (II) where R1 and A are each as defined above, in the presence of at least one catalyst, which comprises converting said nitrile II into an oligomer mixture, and treating with superheated steam.

Abstract translation: 本公开是制备式I的环状内酰胺的方法：其中R 1是氢，烷基，环烷基或芳基，A是未被取代或被1,2,3,4,5或6个取代基取代的C 3 -C 12亚烷基， 通过在至少一种催化剂的存在下，通过转化式II的ω-氨基腈（其中R 1和A各自如上所定义），其中包括将所述腈II 进入低聚物混合物，并用过热蒸汽处理。

公开(公告)号：US06207827B1

公开(公告)日：2001-03-27

申请号：US09295310

申请日：1999-04-21

Applicant: Rudolf P. M. Guit

Inventor： Rudolf P. M. Guit

IPC: C07D20116

CPC classification number: C07D201/16 ,  C07D201/08

Abstract: Process to separate &egr;-caprolactam from 6-aminocaproamide and 6-aminocaproamide oligomers, wherein &egr;-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 &egr;-caprolactam and an alcohol phase which is rich in &egr;-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离的方法，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，得到 第一水性萃余相，其ε-己内酰胺不良和富含ε-己内酰胺且醇相含有6-氨基己酰胺和/或6-氨基己酰胺低聚物的醇相，其中后一个醇相随后与水接触（反冲洗 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：US06204379B1

公开(公告)日：2001-03-20

申请号：US09269875

申请日：1999-07-27

Applicant: Carl Patois ,  Michel Spagnol

Inventor： Carl Patois ,  Michel Spagnol

IPC: C07D20108

CPC classification number: C07D201/08 ,  Y02P20/52

Abstract: The present invention concerns the aminomethylation of pentenoic acid derivatives, by reaction with carbon monoxide, hydrogen and ammonia, for preparing caprolactam. More precisely, it is directed to a method for preparing caprolactam wherein the aminomethylation of pentenoic acid derivatives is carried out by reaction with carbon monoxide, hydrogen, and ammonia, at a temperature higher than 30° C. and in the presence of a catalyst with a base of at least one metal of Group VIII of the Periodic Table.

Abstract translation: 本发明涉及通过与一氧化碳，氢和氨的反应制备己内酰胺的戊烯酸衍生物的氨基甲基化。 更精确地，涉及一种制备己内酰胺的方法，其中戊烯酸衍生物的氨基甲基化通过与一氧化碳，氢气和氨在高于30℃的温度下反应并在催化剂存在下进行， 元素周期表第Ⅷ族至少一种金属的碱。

公开(公告)号：US06194572B1

公开(公告)日：2001-02-27

申请号：US09376310

申请日：1999-08-18

Applicant: Wim Buijs ,  Henricus F. W. Wolters ,  Rudolf P. M. Guit ,  Frank P. W. Agterberg

Inventor： Wim Buijs ,  Henricus F. W. Wolters ,  Rudolf P. M. Guit ,  Frank P. W. Agterberg

IPC: C07D20108

CPC classification number: C07D201/08

Abstract: Process to prepare &egr;-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 &egr;-caprolactam and steam is obtained, wherein the process is carried out in the absence of a catalyst at a temperature between 250 and 400° C. and at a pressure of between 0.5 and 2 MPa. The invention also encompasses a process to prepare &egr;-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随后的步骤从6-氨基己腈开始制备ε-己内酰胺的方法。

公开(公告)号：US6147208A

公开(公告)日：2000-11-14

申请号：US91130

申请日：1998-06-16

Applicant: Gunther Achhammer ,  Peter Bassler ,  Rolf Fischer ,  Eberhard Fuchs ,  Hermann Luyken ,  Werner Schnurr ,  Guido Voit ,  Lutz Hilprecht

Inventor： Gunther Achhammer ,  Peter Bassler ,  Rolf Fischer ,  Eberhard Fuchs ,  Hermann Luyken ,  Werner Schnurr ,  Guido Voit ,  Lutz Hilprecht

IPC: C07C209/48 ,  C07C209/86 ,  C07C211/12 ,  C07D201/08 ,  C07D201/02

CPC classification number: C07D201/08 ,  C07C209/48 ,  Y02P20/52

Abstract: Caprolactam and hexamethylenediamine are prepared simultaneously starting from adiponitrile.

Abstract translation: PCT No.PCT / EP96 / 05521 Sec。 371日期：1998年6月16日 102（e）日期1998年6月16日PCT 1996年12月11日PCT公布。 公开号WO97 / 23454 日期1997年7月3日由己二腈起始制备己内酰胺和六亚甲基二胺。

公开(公告)号：US6107508A

公开(公告)日：2000-08-22

申请号：US282508

申请日：1999-03-31

Applicant: Jiacheng Zhou ,  Lynette May Oh ,  Philip Ma

Inventor： Jiacheng Zhou ,  Lynette May Oh ,  Philip Ma

IPC: C07D261/08 ,  C07B61/00 ,  C07C253/00 ,  C07C255/17 ,  C07C255/40 ,  C07D201/08 ,  C07D207/04 ,  C07D211/60 ,  C07D265/30 ,  C07D279/10

CPC classification number: C07C253/00 ,  C07D201/08

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：US6100396A

公开(公告)日：2000-08-08

申请号：US230588

申请日：1999-04-23

Applicant: Hubert Gayet ,  Philippe Leconte ,  Philippe Perrona

Inventor： Hubert Gayet ,  Philippe Leconte ,  Philippe Perrona

IPC: C07D203/16 ,  C07C253/34 ,  C07D201/08 ,  C07D201/16

CPC classification number: C07D201/16 ,  C07C253/34 ,  C07D201/08

Abstract: A method for purifying lactams by liquid-liquid extraction and/or processing with an ion exchange resin is disclosed. The method is useful for purifying lactams produced by the cyclising vapour-phase hydrolysis of an aliphatic aminonitrile, and comprises removing the major part of the ammonia before subjecting the lactam to liquid-liquid extraction by means of a solvent including an acidic solvent and/or contacting said lactam with a cation exchange resin. In most applications of the lactam, it is preferable to carry out a hydrogenation step on the compounds of the lactam solution comprising unsaturations, prior to or in addition to the liquid-liquid extraction step and/or the acidic resin contact step. The purification method may also include an oxidation step in addition to or instead of the hydrogenation step. Said method is preferably combined with a distillation step in the presence of a base.

Abstract translation: PCT No.PCT / FR97 / 01426 Sec。 371日期1999年4月23日第 102（e）1999年4月23日PCT PCT 1997年7月31日PCT公布。 公开号WO98 / 05636 日期1998年2月12日公开了通过液 - 液萃取和/或用离子交换树脂处理来提纯内酰胺的方法。 该方法可用于纯化通过脂族氨基腈的气相汽相水解产生的内酰胺，并且包括在将内酰胺进行液 - 液萃取之前，通过包括酸性溶剂和/或 使所述内酰胺与阳离子交换树脂接触。 在内酰胺的大多数应用中，优选在液 - 液萃取步骤和/或酸性树脂接触步骤之前或之后对包含不饱和的内酰胺溶液的化合物进行氢化步骤。 除了氢化步骤之外或代替氢化步骤，纯化方法还可以包括氧化步骤。 所述方法优选在碱的存在下与蒸馏步骤组合。