公开(公告)号：US5874575A

公开(公告)日：1999-02-23

申请号：US725438

申请日：1996-10-03

Applicant: Eberhard Fuchs ,  Guenther Achhammer

Inventor： Eberhard Fuchs ,  Guenther Achhammer

IPC: C07D201/08 ,  C07D223/10 ,  B01D3/00

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

Abstract: An improved process for the preparation of caprolactam by heating 6-aminocapronitrile in the presence of a heterogenous catalyst and water under superatmospheric pressure without rapid deactivation of the catalysts used. The process further includes the addition of a low or high boiling alcohol in the heating phase, after which the products are obtained by distillation. The process further includes a method of working up the top and bottom products of the reactors to achieve higher yields.

Abstract translation: 通过在异丙烯催化剂和水的存在下，在超大气压下加热6-氨基己腈而不快速失活所用催化剂制备己内酰胺的改进方法。 该方法还包括在加热阶段加入低沸点或高沸点醇，之后通过蒸馏获得产物。 该方法还包括处理反应器的顶部和底部产物以实现更高产率的方法。

公开(公告)号：US5717090A

公开(公告)日：1998-02-10

申请号：US565214

申请日：1995-11-30

Applicant: Peter Bassler ,  Hermann Luyken ,  Gunther Achhammer ,  Tom Witzel ,  Eberhard Fuchs ,  Rolf Fischer ,  Werner Schnurr

Inventor： Peter Bassler ,  Hermann Luyken ,  Gunther Achhammer ,  Tom Witzel ,  Eberhard Fuchs ,  Rolf Fischer ,  Werner Schnurr

IPC: C07D201/08

CPC classification number: C07D201/08

Abstract: Caprolactam and hexamethylenediamine are prepared simultaneously starting from adiponitrile by a process in which (a) adiponitrile is partially hydrogenated to give a mixture containing essentially 6-aminocapronitrile, hexamethylenediamine, ammonia, adiponitrile and hexamethyleneimine, (b) the mixture obtained in (a) is subjected to a distillation to give ammonia as the top product and a bottom product I, (c) the bottom product I containing essentially 6-aminocapronitrile, hexamethylenediamine, adiponitrile, hexamethyleneimine, inert compound A and ammonia, the ammonia content being lower than that of the mixture used in stage (b), is subjected to a second distillation to give a mixture comprising the inert compound A and ammonia as the top product and a bottom product II, (d) the bottom product II is subjected, in a third column, to a distillation to give the inert compound A as the top product and a bottom product III, (e) the bottom product III is subjected, in a fourth column, to a distillation to give a top product KP1, containing essentially hexamethyleneimine and a bottom product IV, (f) the top product KP1 is subjected, in a fifth column, to a distillation to give a top product KP2, which contains essentially hexamethyleneimine, and (g) the bottom product IV containing essentially 6-aminocapronitrile and adiponitrile is subjected, in a sixth column, to a distillation to give 6-aminocapronitrile, and the 6-aminocapronitrile thus obtained is then cyclized to give caprolactam.

Abstract translation: 己二醇和六亚甲基二胺由己二腈通过以下方法同时制备，其中（a）己二腈部分氢化得到基本上含有6-氨基己腈，六亚甲基二胺，氨，己二腈和六亚甲基亚胺的混合物，（b）将（a）中得到的混合物 进行蒸馏以产生氨作为顶部产物，底部产物I，（c）含有基本上为6-氨基己腈，六亚甲基二胺，己二腈，六亚甲基亚胺，惰性化合物A和氨的底部产物I，氨含量低于 将阶段（b）中使用的混合物进行第二次蒸馏，得到包含惰性化合物A和氨作为顶部产物的混合物和底部产物II，（d）底部产物II经受第三塔 进行蒸馏，得到惰性化合物A作为顶部产物和底部产物III，（e）底部产物III在第四列中经受 蒸馏得到基本上为六亚甲基亚胺和底部产物IV的顶部产物KP1，（f）顶部产物KP1在第五个塔中进行蒸馏，得到基本上含有六亚甲基亚胺的顶部产物KP2，和（g ）将含有基本上6-氨基己腈和己二腈的底部产物IV在第六塔中进行蒸馏以得到6-氨基己腈，然后将所得的6-氨基己腈环化，得到己内酰胺。

公开(公告)号：US5700934A

公开(公告)日：1997-12-23

申请号：US616742

申请日：1996-03-15

Applicant: Henricus F. W. Wolters ,  Samuel L. Lane ,  Wim Buijs ,  Nicolaas F. Haasen ,  Frank E. Herkes

Inventor： Henricus F. W. Wolters ,  Samuel L. Lane ,  Wim Buijs ,  Nicolaas F. Haasen ,  Frank E. Herkes

IPC: C07D201/08

CPC classification number: C07D201/08

Abstract: A process for the preparation of .epsilon.-caprolactam and .epsilon.-caprolactam precursors, starting from the corresponding 5-formylvalerate ester, ammonia and hydrogen in the presence of a hydrogenation catalyst is disclosed, wherein in a step (a) 5-formylvalerate ester is reacted with ammonia under non-hydrogenating conditions, and in a step (b) the reaction product obtained in step (a) is converted to .epsilon.-caprolactam and the .epsilon.-caprolactam precursor(s) under hydrogenating conditions, in the presence of ammonia.

Abstract translation: 公开了在氢化催化剂存在下从相应的5-甲酰基戊酸酯，氨和氢开始制备ε-己内酰胺和ε-己内酰胺前体的方法，其中在步骤（a）中，使5-甲酰基戊酸酯反应 在非氢化条件下用氨，并且在步骤（b）中，在氨的存在下，在氢化条件下将步骤（a）中获得的反应产物转化成ε-己内酰胺和ε-己内酰胺前体。

公开(公告)号：US5276165A

公开(公告)日：1994-01-04

申请号：US982300

申请日：1992-11-25

Applicant: Hans-Juergen Weyer ,  Rolf Fischer

Inventor： Hans-Juergen Weyer ,  Rolf Fischer

IPC: B01J21/04 ,  B01J23/28 ,  B01J23/34 ,  B01J23/72 ,  B01J23/75 ,  C07B61/00 ,  C07D201/02 ,  C07D201/08 ,  C07D207/26 ,  C07D207/267 ,  C07D209/46 ,  C07D209/64 ,  C07D223/10 ,  C07D225/02 ,  C07D207/12 ,  C07D221/06

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

Abstract: A process for the preparation of N-substituted lactams of the formula I ##STR1## where Z is C.sub.2 - to C.sub.10 -alkylene, C.sub.7 - to C.sub.12 -aralkylene, phenylene or naphthylene, andR.sup.1 is C.sub.1 - to C.sub.20 -alkyl, C.sub.6 - to C.sub.10 -aryl or C.sub.7 - to C.sub.12 -aralkyl,by hydrogenating a compound of the formula II ##STR2## where W is C.sub.2 - to C.sub.10 -alkylene, C.sub.2 - to C.sub.10 -alkenylene, C.sub.7 - to C.sub.12 -aralkylene, phenylene or naphthylene, andX and Y together form an oxa or imido bridge of the formula ##STR3## or alternatively are identical or different and are hydroxyl, C.sub.1 - to C.sub.20 -alkoxy, C.sub.6 - to C.sub.10 -aryloxy or C.sub.7 - to C.sub.12 -aralkoxy, and, if X and Y are different, Y, in addition to the abovementioned meanings, may also be hydrogen,at superatmospheric pressure and at elevated temperature in the presence of a catalyst and in the presence of an amine, which comprises using a secondary and/or tertiary amine of the formula IIINH.sub.n R.sub.3-n .sup.1where R.sup.1 is as defined above and n is 0 or 1, or a mixture of a secondary and/or teritary amine of this type with a primary amine of the formula IVR.sup.1 --NH.sub.2 (IV)as the starting material, and carrying out the reaction with addition of water and/or ammonia.

Abstract translation: 制备式I的N-取代的内酰胺的方法（I）其中Z为C 2至C 10亚烷基，C 7至C 12 - 亚芳基，亚苯基或亚萘基，R 1为C 1 -C 20烷基 C 6 -C 10 - 芳基或C 7 - 至C 12 - 芳烷基，其中W是C 2 - 至C 10 - 亚烷基，C 2至C 10亚烯基，C 7 - 至C 12 - 亚烷基， - 亚烷基，亚苯基或亚萘基，X和Y一起形成下式的氧杂或亚氨基桥，或者可选地相同或不同，为羟基，C 1至C 20 - 烷氧基，C 6至C 10 - 芳氧基或C 7 - 对于C 12 - 芳烷氧基，并且如果X和Y不同，除了上述含义之外，Y还可以是氢，在超大气压和升高的温度下，在催化剂的存在下和在胺的存在下， 包括使用式III NH n R 3-n 1的仲和/或叔胺，其中R 1如上定义并且n为0或1，或者该仲胺和/或叔胺的混合物 以式ⅣR-NH2（Ⅳ）的伯胺为起始原料，并加入水和/或氨进行反应。

公开(公告)号：US4767857A

公开(公告)日：1988-08-30

申请号：US133735

申请日：1987-12-16

Applicant: Franz Merger ,  Claus-Ulrich Priester ,  Rolf Fischer ,  Manfred Sauerwald

Inventor： Franz Merger ,  Claus-Ulrich Priester ,  Rolf Fischer ,  Manfred Sauerwald

IPC: C07D201/08

CPC classification number: C07D201/08

Abstract: Caprolactam is prepared by heating a 6-aminocaproic ester at 100.degree.-320.degree. C. in the presence of a reaction medium comprising an aromatic hydrocarbon which is liquid under reaction conditions and has a boiling point from 80.degree. to 240.degree. C., and isolating caprolactam from the reaction medium.

Abstract translation: 在含有在反应条件下为液体并且沸点为80-240℃的芳族烃的反应介质存在下，在100-320℃下加热6-氨基己酸酯制备己内酰胺， 从反应介质中分离己内酰胺。

公开(公告)号：US4730040A

公开(公告)日：1988-03-08

申请号：US7788

申请日：1987-01-28

Applicant: Uwe Vagt ,  Rolf Fischer ,  Franz Merger ,  Hans-Martin Hutmacher

Inventor： Uwe Vagt ,  Rolf Fischer ,  Franz Merger ,  Hans-Martin Hutmacher

IPC: C07D223/04 ,  C07D201/08

CPC classification number: C07D201/08

Abstract: .epsilon.-caprolactam is prepared by a process in which(a) a 5-formylvalerate is reacted with water in the presence of an acidic agent at from 30.degree. to 200.degree. C.,(b) the 5-formylvaleric acid thus obtained is reacted with excess ammonia and hydrogen in the presence of a hydrogenation catalyst and of a solvent which is inert under the reaction conditions, at from 50.degree. to 150.degree. C. under superatmospheric pressure, and(c) after the ammonia has been separated off, the resulting solution of 6-aminocaproic acid is heated to 150.degree.-370.degree. C. and the caprolactam formed is isolated.

Abstract translation: ε-己内酰胺通过以下方法制备：（a）在30℃至200℃下，在酸性试剂存在下，使5-甲酰基戊酸酯与水反应，（b）将所得的5-甲酰基戊酸反应 在氢化催化剂和在反应条件下为惰性的溶剂中，在超大气压下，在50-150℃下，过量的氨和氢，和（c）氨分离后， 将得到的6-氨基己酸溶液加热至150-370℃，形成己内酰胺。

公开(公告)号：US4647661A

公开(公告)日：1987-03-03

申请号：US845122

申请日：1986-03-27

Applicant: Paolo Senni ,  Leandro Zuliani ,  Sergio Ferruzzi

Inventor： Paolo Senni ,  Leandro Zuliani ,  Sergio Ferruzzi

IPC: C07D201/16 ,  C07D201/08 ,  C07D201/10

CPC classification number: C07D201/08

Abstract: A method of preparing .omega.-lactams, in particular caprolactam, comprising: a step of premixing cycloaliphatic acids having the formula ##STR1## where n=3-13, with a dehydrating agent; the first step of reaction with a nitrosating agent; the second step of reaction with the addition of a very small amount of water corresponding to a molar ratio U=H.sub.2 O/SO.sub.3 within the 0.1 to 0.9 range; and the step of reclaiming the unreacted cycloaliphatic acid. The method affords improved output from the lactamization reaction and reduced byproducts.

Abstract translation: 一种制备ω-内酰胺，特别是己内酰胺的方法，包括：将具有式“IMAGE”的其中n = 3-13的脂环族酸与脱水剂预混合的步骤; 与亚硝化剂反应的第一步; 反应的第二步骤是加入相当于0.1至0.9范围内的摩尔比U = H 2 O / SO 3的非常少量的水; 以及回收未反应的脂环族酸的步骤。 该方法提供了来自内酰胺化反应的改进的产物和减少的副产物。

公开(公告)号：US4625023A

公开(公告)日：1986-11-25

申请号：US771853

申请日：1985-09-03

Applicant: Frank Mares ,  Reginald Y. Tang ,  James E. Galle ,  Rose M. Federici

Inventor： Frank Mares ,  Reginald Y. Tang ,  James E. Galle ,  Rose M. Federici

IPC: C07D201/08 ,  C07D223/10

CPC classification number: C07D201/08

Abstract: Process for the selective conversion of dinitriles into the corresponding lactam by treating the dinitrile with an effective amount of a hydrogenation catalyst such as copper chromite in combination with a co-catalyst, such as titania, at a temperature in the range of from about 200.degree. C. to about 400.degree. C. and at a pressure of at least 50 kPa in the presence of water and hydrogen.

Abstract translation: 通过用有效量的氢化催化剂如亚铬酸铜与助催化剂如二氧化钛的组合处理二腈，将二腈选择性转化成相应的内酰胺的方法，温度范围为约200℃ 在约400℃下和在水和氢气存在下在至少50kPa的压力下进行。

公开(公告)号：US4599199A

公开(公告)日：1986-07-08

申请号：US696796

申请日：1985-01-31

Applicant: Hugo Fuchs

Inventor： Hugo Fuchs

IPC: C07D201/08

CPC classification number: C07D201/08

Abstract: Caprolactam is obtained by treating .epsilon.-aminocaproic acid with steam at elevated temperatures in the presence of a catalyst by a process in whcih .epsilon.-aminocaproic acid is introduced into a fluidized alumina bed and treated in the presence of steam at from 290.degree. to 400.degree. C.

Abstract translation: 己内酰胺通过在催化剂存在下在高温下用蒸汽处理ε-氨基己酸获得，其中将ε-氨基己酸引入流化的氧化铝床中并在290°至400°的蒸气存在下进行处理 C。

公开(公告)号：US4518602A

公开(公告)日：1985-05-21

申请号：US537862

申请日：1983-09-30

Applicant: Shinji Terao ,  Kohei Nishikawa

Inventor： Shinji Terao ,  Kohei Nishikawa

IPC: C07C51/363 ,  C07D201/08 ,  C07D213/26 ,  C07D213/30 ,  C07D213/32 ,  C07D213/50 ,  C07D213/55 ,  C07D213/57 ,  C07D405/06 ,  C07D409/04 ,  C07D409/06 ,  C07F9/54 ,  A61K31/44 ,  C07D211/82 ,  C07D407/06

CPC classification number: C07D213/30 ,  C07C51/363 ,  C07D201/08 ,  C07D213/26 ,  C07D213/32 ,  C07D213/50 ,  C07D213/55 ,  C07D213/57 ,  C07D405/06 ,  C07D409/04 ,  C07D409/06 ,  C07F9/5407

Abstract: Novel compound of the formula: ##STR1##wherein R.sup.1 is a pyridyl group; R.sup.2 is a phenyl, thienyl, furyl, naphthyl, benzothienyl or pyridyl group which may have as a substituent a lower alkoxy, a lower alkyl, a halogen, trifluoromethyl, a lower alkenyl or methylenedioxy; R.sup.3 is hydrogen, benzyl or a lower alkyl; one of R.sup.4 and R.sup.5 is hydrogen or a lower alkyl, and the other is an aryloxy, or lower aliphatic hydrocarbon, an alicyclic hydrocarbon having not more than 6 carbon atoms or an aromatic group which may have a substituent, or a group represented by the formula, --S(O).sub.m --R.sup.6 (in which R.sup.6 is phenyl or a lower alkyl group; m is an integer of 0 to 2), or R.sup.4 and R.sup.5 each combine with the other to represent one alkylene group; n is an integer of 2 to 6, or a pharmaceutically acceptable salt thereof has a selective inhibitory action on bio-synthesis of thromboxane A.sub.2 (TXA.sub.2) and an effect of enhancing the production of prostaglandin I.sub.2 (PGI.sub.2), and can be used in mammals for to prevention and treatment of arterial thrombosis caused by platelet aggregation or ischemic diseases caused by vasospasms in cardiac, cerebral and peripheral circulatory system (e.g. cardian infarction, apoplexy, infarct of blood vessels in kidney, lung and other organs, pectic ulcer, etc.).

Abstract translation: 下式的新型化合物：其中R 1是吡啶基; R2是可以具有低级烷氧基，低级烷基，卤素，三氟甲基，低级烯基或亚甲二氧基的取代基的苯基，噻吩基，呋喃基，萘基，苯并噻吩基或吡啶基。 R3是氢，苄基或低级烷基; R4和R5中的一个是氢或低级烷基，另一个是芳氧基或低级脂族烃，不大于6个碳原子的脂环族烃或可以具有取代基的芳族基团，或由 式（-S（O）m -R 6（其中R 6为苯基或低级烷基; m为0〜2的整数），或者R 4和R 5各自与一个亚烷基结合， n为2〜6的整数，或其药学上可接受的盐对凝血恶烷A2（TXA2）的生物合成具有选择性抑制作用和增强前列腺素I2（PGI2）的产生的作用，可用于哺乳动物 用于预防和治疗由心脏，脑和周围循环系统（例如心脏梗塞，中风，肾脏，肺部和其他器官中的血管梗死，果胶性溃疡等）引起的血小板聚集或血管痉挛引起的缺血性疾病引起的动脉血栓形成。 ）。