公开(公告)号：US06858728B2

公开(公告)日：2005-02-22

申请号：US10464104

申请日：2003-06-17

Applicant: Gregory S. Kirby ,  John J. Ostermaier

Inventor： Gregory S. Kirby ,  John J. Ostermaier

IPC: C07D201/08 ,  C07D201/00 ,  C07D201/02

CPC classification number: C07D201/08

Abstract: Method for making caprolactam from 6-aminocapronitrile that contains greater than 500 ppm tetrahydroazepine and its derivatives (THA) in which the THA is not removed from the method until after the caprolactam is produced.

Abstract translation: 从6-氨基己腈制备己内酰胺的方法，其含有大于500ppm的四氮氮平及其衍生物（THA），其中THA不从该方法中除去，直到己内酰胺生产。

公开(公告)号：US06835830B1

公开(公告)日：2004-12-28

申请号：US09720598

申请日：2001-05-07

Applicant: Gerald Bocquenet ,  Henri Chiarelli ,  Philippe Leconte

Inventor： Gerald Bocquenet ,  Henri Chiarelli ,  Philippe Leconte

IPC: C07D201108

CPC classification number: C07D201/08

Abstract: The invention concerns a method for evaporating aminonitrile and water in conditions limiting or eliminating the formation of heavy by-products in particular amino-carboxylic acid oligomers. To avoid said inconvenience, said method for evaporating aminonitrile and water is characterised in that the water in vapour state serves as balance gas for evaporation.

Abstract translation: 本发明涉及在限制或消除特别是氨基羧酸低聚物形成重质副产物的条件下蒸发氨腈和水的方法。 为了避免所述不便，所述蒸发氨腈和水的方法的特征在于，蒸汽状态的水用作蒸发的平衡气体。

公开(公告)号：US06794553B2

公开(公告)日：2004-09-21

申请号：US10287731

申请日：2002-11-04

Applicant: Eit Drent ,  Michael Rolf Eberhard ,  Paul Gerald Pringle ,  Renata Helena van der Made

Inventor： Eit Drent ,  Michael Rolf Eberhard ,  Paul Gerald Pringle ,  Renata Helena van der Made

IPC: C07C132

CPC classification number: B01J31/248 ,  B01J23/44 ,  B01J31/1895 ,  B01J31/24 ,  B01J2231/20 ,  B01J2531/80 ,  B01J2531/824 ,  C07C2/36 ,  C07C2/406 ,  C07C41/06 ,  C07C253/30 ,  C07C2531/24 ,  C07C2531/28 ,  C07D201/08 ,  C07F9/5027 ,  C07F9/65683 ,  C07C255/19 ,  C07C11/12 ,  C07C43/15

Abstract: Process for the telomerization of a conjugated diene, wherein the conjugated diene is reacted with a compound containing an active hydrogen atom and having a formula R′—H in the presence of a telomerization catalyst based on: (a) a source of group VIII metal, (b) a bidentate ligand wherein the bidentate ligand has the general formula I R1R2M1—R—M2R3R4  (I) wherein M1 and M2 are independently P, As or Sb; R1, R2, R3 and R4 independently represent a monovalent aliphatic group; or R1, R2 and M1 together and/or R3, R4 and M2 together independently represent an optionally substituted aliphatic cyclic group with at least 5 ring atoms, of which one is the M1 or M2 atom, respectively; R represents a bivalent organic bridging group; and novel bidentate diphosphines which can be used in this process.

Abstract translation: 共轭二烯的调聚方法，其中在调聚催化剂的存在下，共轭二烯与含有活性氢原子的化合物反应并具有式R'-H，其基于：（a）VIII族金属源 ，（b）二齿配位体中的二齿配位体具有通式I，其中M 1和M 2独立地为P，As或Sb; R 1，R 2，R 3和R 4 >独立地表示一价脂族基团;或R 1，R 2和M 1一起和/或R 3，R 4和M 2一起独立地表示任选取代的脂族环基 具有至少5个环原子，其中一个是M 1或M 2原子; R代表二价有机桥基; 和可用于该方法的新型二齿二膦。

公开(公告)号：US20040171829A1

公开(公告)日：2004-09-02

申请号：US10786992

申请日：2004-02-25

Applicant: Bristol-Myers Squibb Pharma Company

Inventor： Jiacheng Zhou ,  Lynette May Oh ,  Philip Ma

IPC: C07D279/12 ,  C07D265/30 ,  C07D211/06 ,  C07D241/04

CPC classification number: C07D261/10 ,  C07C253/00 ,  C07C255/41 ,  C07D201/08 ,  C07D261/08 ,  Y10S977/915 ,  C07C255/17 ,  C07C255/40

Abstract: The present invention relates to processes for the production of null-aryl-null-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：US20040132999A1

公开(公告)日：2004-07-08

申请号：US10473077

申请日：2004-02-27

Inventor： Wim Buijs ,  Henricus Franciscus Wilhelmus

IPC: C07D201/02

CPC classification number: C08G69/16 ,  C07D201/08

Abstract: The invention relates to a process for the preparation of null-caprolactam starting from 6-aminocapronitrile by hydrolysis/oligomerisation followed by de-oligomerisation/cyclisation using superheated steam characterized in that the hydrolysis/oligomerisation is performed with superheated steam converting 6-aminocapronitrile into a molten phase and a gas phase comprising ammonia, ammonia is continuously separated off and the de-oligomerisation/cyclisation is performed by treating the molten phase further with superheated steam. The invention also relates to a process for the preparation of null-caprolactam starting from 6-aminocapronitrile by hydrolysis/oligomerisation followed by de-oligomerisation/cyclisation characterized in that the preparation is performed in a horizontal scraped-surface reactor, the hydrolysis/oligomerisation is performed with superheated steam converting 6-aminocapronitrile into a molten phase and a gas phase comprising ammonia, ammonia is continuously separated off and the de-oligomerisation/cyclisation is performed by treating the molten phase further with superheated steam.

Abstract translation: 本发明涉及一种从6-氨基己腈开始通过水解/低聚制备ε-己内酰胺的方法，然后使用过热蒸汽进行脱低聚/环化，其特征在于水解/低聚反应用过热蒸汽将6-氨基己腈转化成 熔融相和包含氨的气相，氨被连续分离，并且通过用过热蒸汽进一步处理熔融相进行脱低聚/环化。 本发明还涉及从6-氨基己腈开始制备ε-己内酰胺的方法，其通过水解/低聚，接着进行脱低聚/环化，其特征在于制备在水平刮面反应器中进行，水解/低聚是 使用过热蒸汽将6-氨基己腈转化成熔融相和包含氨的气相，连续分离氨，通过用过热蒸汽进一步处理熔融相进行脱低聚/环化。

公开(公告)号：US06686465B2

公开(公告)日：2004-02-03

申请号：US10258943

申请日：2002-10-29

Applicant: Frank Ohlbach ,  Andreas Ansmann ,  Peter Bassler ,  Rolf-Hartmuth Fischer ,  Hermann Luyken ,  Stefan Maixner ,  Johann-Peter Melder

Inventor： Frank Ohlbach ,  Andreas Ansmann ,  Peter Bassler ,  Rolf-Hartmuth Fischer ,  Hermann Luyken ,  Stefan Maixner ,  Johann-Peter Melder

IPC: C07D20108

CPC classification number: C07D201/08

Abstract: A process is provided for the preparation of cyclic lactams of formula (II): in which n and m can each have the values 0, 1, 2, 3, 4, 5, 6, 7, 8 and 9 and the sum of n+m is at least 3, preferably at least 4, and R1 and R2 are C1-C6-alkyl, C5-C7-cycloalkyl or C6-C12-aryl groups, by reacting a compound (I) of the formula in which R1, R2, m and n are as defined above and R are [sic] nitrile, carboxamide and carboxylic acid groups, with steam in the gas phase.

Abstract translation: 提供了制备式（II）的环状内酰胺的方法：其中n和m各自可以具有0,1,2,3,4,5,6,7,8和9以及n + m为至少3，优选至少4，R 1和R 2为C 1 -C 6 - 烷基，C 5 -C 7 - 环烷基或C 6 -C 12 - 芳基，通过使 R 1，R 2，m和n如上所定义，R是具有气相中蒸汽的[sic]腈，甲酰胺和羧酸基团的甲醛。

公开(公告)号：US06683180B2

公开(公告)日：2004-01-27

申请号：US10297209

申请日：2002-12-04

Applicant: Frank Ohlbach ,  Andreas Ansmann ,  Rolf-Hartmuth Fischer ,  Johann-Peter Melder

Inventor： Frank Ohlbach ,  Andreas Ansmann ,  Rolf-Hartmuth Fischer ,  Johann-Peter Melder

IPC: C07D20108

CPC classification number: C07D201/08 ,  Y02P20/52

Abstract: A process is provided for the preparation of caprolactam from a compound of formula (I): NC—(CH2)5—CO—R  (I) in which R is a carboxamide, carboxylic acid or carboxylic acid ester group, wherein a) a compound (I) or a mixture of such compounds, in the presence of ammonia and optionally a liquid diluent (VI), is hydrogenated with hydrogen in the presence of a catalyst (II) to give a mixture (III), b) the hydrogen and the catalyst (II) are separated from the mixture (III) to give a mixture (IV), and c) the mixture (IV), optionally in the presence of a liquid diluent (VII), is converted to caprolactam in the presence of a catalyst (V).

Abstract translation: 提供了从式（I）化合物制备己内酰胺的方法：其中R是羧酰胺，羧酸或羧酸酯基，其中a）化合物（I）或这些化合物的混合物，在存在下 的氨和任选的液体稀释剂（VI）在催化剂（II）的存在下用氢氢化，得到混合物（III），b）将氢气和催化剂（II）从混合物（III）中分离出来， 任选在液体稀释剂（VII）的存在下，将混合物（IV）和（c）混合物（IV）在催化剂（V）的存在下转化成己内酰胺。

公开(公告)号：US20040014965A1

公开(公告)日：2004-01-22

申请号：US10296512

申请日：2003-07-30

Inventor： Daniel Amoros ,  Philippe Leconte ,  Pierre Coqueret

IPC: C07D21/08 ,  C07D21/16

CPC classification number: C07D201/16 ,  C07D201/08 ,  Y10S203/90

Abstract: The invention concerns a method for purifying lactams, more particularly lactams obtained by cyclizing hydrolysis of aminonitrile. More particularly, the invention concerns the purification of null-caprolactam obtained by cyclizing hydrolysis of aminocapronitrile which consists in eliminating the ammonia from the reaction medium of the hydrolysis then in recuperating the lactam from said medium in purified form. Said recuperation is carried out by performing at least a distillation of the lactam in the presence of a base producing optionally a fronts fraction comprising compounds more volatile than the lactam, a fraction comprising the lactam to be recuperated to the degree of desired purity and a distillation tails comprising the lactam and compounds less volatile than the lactam. The distillation tails are treated by various processes such as evaporation in thin layers to recuperate the major part of the comprised caprolactam and recycling the latter in the purification process. The invention enables a high rate of recuperation of the caprolactam contained in the hydrolysis medium, while observing the required criteria of purity.

Abstract translation: 本发明涉及一种纯化内酰胺的方法，更特别的是通过环化氨基腈的水解得到的内酰胺。 更具体地说，本发明涉及通过环化氨基己腈的水解而得到的ε-己内酰胺的纯化，其包括从水解反应介质中除去氨，然后将内酰胺从纯化形式的所述培养基中回收。 所述的回收是通过在碱的存在下至少进行内酰胺的蒸馏来进行的，所述碱产生任选地含有比内酰胺更易挥发的化合物的前列馏分，包含待还原的内酰胺至所需纯度的馏分和蒸馏 尾部包含内酰胺和化合物比内酰胺更不易挥发。 蒸馏尾部通过各种方法处理，例如在薄层中蒸发以回收主要部分的己内酰胺并在净化过程中再循环。 本发明能够在观察所需的纯度标准的同时高效地回收水解介质中所含的己内酰胺。

公开(公告)号：US20030153749A1

公开(公告)日：2003-08-14

申请号：US10297209

申请日：2002-12-04

Inventor： Frank Ohlbach ,  Andreas Ansmann ,  Rolf-Hartmuth Fischer ,  Johann-Peter Melder

IPC: C07D201/02

CPC classification number: C07D201/08 ,  Y02P20/52

Abstract: A process is provided for the preparation of caprolactam from a compound of formula (I): NCnull(CH2)5nullCOnullRnullnull(I)in which R is a carboxamide, carboxylic acid or carboxylic acid ester group, wherein a) a compound (I) or a mixture of such compounds, in the presence of ammonia and optionally a liquid diluent (VI), is hydrogenated with hydrogen in the presence of a catalyst (II) to give a mixture (III), b) the hydrogen and the catalyst (II) are separated from the mixture (III) to give a mixture (IV), and c) the mixture (IV), optionally in the presence of a liquid diluent (VII), is converted to caprolactam in the presence of a catalyst (V).

Abstract translation: 提供了从式（I）化合物制备己内酰胺的方法：NC-（CH 2）5 -CO-R（I），其中R是羧酰胺，羧酸或羧酸酯基，其中a） 在氨和任选的液体稀释剂（VI）存在下，化合物（I）或这些化合物的混合物在氢气存在下在催化剂（II）的存在下氢化，得到混合物（III），b）氢 并将催化剂（II）与混合物（III）分离，得到混合物（Ⅳ），和c）任选在液体稀释剂（Ⅶ）存在下，混合物（Ⅳ）在存在下转化为己内酰胺 的催化剂（V）。

公开(公告)号：US20030132098A1

公开(公告)日：2003-07-17

申请号：US10297051

申请日：2002-12-02

Inventor： Hermann Luyken ,  Frank Ohlbach ,  Stefan Maixner ,  Rolf-Hartmuth Fischer ,  Johann-Peter Melder ,  Peter Bassler ,  Andreas Ansmann

IPC: B01D003/00 ,  C01C001/10 ,  B01D005/00

CPC classification number: C01C1/10 ,  C07D201/08 ,  C07D201/16

Abstract: A process for distillative removal of ammonia from solutions (I) which include a lactam and ammonia comprises effecting said removal in a distillation apparatus (a) at an absolute pressure of less than 10 bar.

Abstract translation: 从包括内酰胺和氨的溶液（I）中蒸馏除去氨的方法包括在绝对压力小于10巴的蒸馏装置（a）中进行所述除去。