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    Production of caprolactam starting with cyclohexanone
    61.
    发明授权
    Production of caprolactam starting with cyclohexanone 失效
    生产使用环己酮的起始物起始

    公开(公告)号：US3562254A

    公开(公告)日：1971-02-09

    申请号：US3562254D

    申请日：1969-04-24

    Applicant: TECHNI CHEM CO THE

    Inventor： SHEEHAN DESMOND ,  VELLTURO ANTHONY F ,  GAY WALTER A ,  HEGARTY WILLIAM P ,  THRELKELD DONALD D

    IPC: C07D201/02 ,  C07D41/06

    CPC classification number: C07D201/02

    Abstract: A CONTINUOUS PROCESS FOR THE PRODUCTION OF CAPROLACTAM, INCLUDING ACETYLATION OF CYCLOHEXANONE WITH ACETIC ANHYDRIDE AND KETENE (WHICH REACTS WITH ACETIC ACID FORMED IN THE ACETYLATION REACTION). THE CYCLOHEXENYL ACETATE FORMED IS THEN NITRATED WITH CONCENTRATED NITRIC ACID AND THE RESULTING NITROCYCLOHEXANONE SEPARATED BY DISTILLATION. ACETIC ANHYDRIDE IS RECYCLED TO THE ACETYLATION REACTION, AND ACETIC ACID TOGETHER WITH MAKEUP ACETIC ACID IS PYROLYZED TO KETENE, WHICH IS ALSO USED IN THE ACETYLATION REACTION. THE NITROCYCLOHEXANONE IS THEN CLEAVED WITH AMMONIUM HYDROXIDE TO FORM THE AMMONIUM SALT OF 6-NITRO CAPROIC ACID, WHICH IS THEN REDUCED WITH HYDROGEN AND A HYDROGENATION CATALYST TO PRODUCE 6-AMINO CAPROIC ACID. THIS INTERMEDIATE IS THEN SEPARATED BY REMOVING AMMONIA, WHICH IS RECYCLED WITH MAKEUP AMMONIA TO THE CLEAVAGE REACTION. THE AQUEOUS 6-AMINO CAPROIC ACID IS THEN HEATED IN DILUTE AQUEOUS SOLUTION, 5% TO 25% W./V., TO CYCLIZE TO CAPROLACTAM. THE CAPROLACTAM IS THEN EXTRACTED WITH AN ORGANIC SOLVENT, SUCH AS TRICHLOROETHYLENE, AND THE UNCONVERTED AQUEOUS AMINO CAPROIC ACID RECYCLE TO THE CYCLIZATION STEP. SOLVENT IS THEN REMOVED AND THE CAPROLACTAM PURIFIED BY KNOWN MEANS. AN IMPORTANT PART OF THE PROCESS IS THAT THERE IS NO AMMONIUM SULFATE FORMED, WHICH IN EARLIER PROCESSES WAS AN UNDESIRABLE BY-PRODUCT. THE AMMONIA USED IN THE CLEAVAGE REACTION IS RECYCLED AND THERE IS NO LARGE LOSS OF RAW MATERIAL.

    Production of Lactams
    65.
    发明申请
    Production of Lactams 失效
    内华达州的生产

    公开(公告)号：US20090234115A1

    公开(公告)日：2009-09-17

    申请号：US11884883

    申请日：2006-02-14

    Applicant: Philippe Leconte

    Inventor： Philippe Leconte

    IPC: C07D201/02

    CPC classification number: C07D201/08 ,  Y02P20/52

    Abstract: Lactams, notably ε-caprolactam, are prepared from alkyl cyanovalerates, themselves obtained from unsaturated nitrile compounds, by contacting same, in gaseous state, with hydrogen in the presence of hydrogenation/cyclization catalysts, and then condensing the gas stream thus formed, without intermediate separation of any alkyl aminocaproate, and recovering lactam produced therefrom.

    Abstract translation: 内酰胺，特别是ε-己内酰胺，由本身由不饱和腈化合物获得的烷基氰基戊酸酯通过在氢化/环化催化剂存在下以气态与氢气接触而制备，然后将如此形成的气流冷凝而无中间体 分离任何烷基氨基己酸酯，并回收由其制备的内酰胺。

    PROCESS FOR THE PREPARATION OF AN N-ALKYL LACTAM WITH IMPROVED COLOUR QUALITY
    66.
    发明申请
    PROCESS FOR THE PREPARATION OF AN N-ALKYL LACTAM WITH IMPROVED COLOUR QUALITY 审中-公开
    制备具有改善颜色质量的N-ALKYL LACTAM的方法

    公开(公告)号：US20090182139A1

    公开(公告)日：2009-07-16

    申请号：US12296115

    申请日：2007-03-29

    Applicant: Tobias Wabnitz ,  Rolf Pinkos ,  Karl Ott

    Inventor： Tobias Wabnitz ,  Rolf Pinkos ,  Karl Ott

    IPC: C07D201/08 ,  C07D207/267 ,  C07D201/02 ,  C07D211/06

    CPC classification number: C07D201/18 ,  C07D207/267 ,  C07D211/76 ,  C07D223/10

    Abstract: A process for preparing an N-alkyllactam with improved color quality, wherein from 0.01 to 10% by weight of a C1-10-alcohol or a compound which releases from 0.01 to 10% by weight of a C1-10-alcohol is added to the N-alkyllactam.A mixture comprising at least 99.0% by weight of an N-alkyllactam and in the range from 100 to 5000 ppm by weight of a C1-10-alcohol or of an acetal, aminal or of an orthoester which releases in the range from 100 to 5000 ppm by weight of a C1-10-alcohol.

    Abstract translation: 一种制备具有改进的颜色质量的N-烷基内酰胺的方法，其中将0.01至10重量％的C 1-10醇或从0.01至10重量％的C 1-10醇释放的化合物加入到 N-烷基内酰胺。 一种混合物，其包含至少99.0重量％的N-烷基内酰胺和100-5000重量ppm的C1-10醇或缩醛，缩醛或原酸酯，其释放范围为100至 5000重量ppm的C 1-10醇。

    Process for making caprolactam
    67.
    发明授权
    Process for making caprolactam 失效
    制备己内酰胺的方法

    公开(公告)号：US07060820B1

    公开(公告)日：2006-06-13

    申请号：US11083728

    申请日：2005-03-18

    Applicant: Sourav K. Sengupta ,  John J. Ostermaier ,  Gregory S. Kirby

    Inventor： Sourav K. Sengupta ,  John J. Ostermaier ,  Gregory S. Kirby

    IPC: C07D201/02

    CPC classification number: C07D201/08

    Abstract: Lactams, in particular ε-caprolactam, are produced by the hydrolytic cyclization of aminonitriles, in particular 6-aminocapronitrile, in the vapor phase in a plurality of adiabatic fixed bed reaction zones arranged in succession wherein at least a portion of the heat of the exothermic reaction is removed between each of the successive reaction zones. Conducting the reaction in such a manner requires less capital for the reactor itself. It has also been found that the product exiting such a reaction system can be directly fed to a distillation unit without the need of additional cooling or storing.

    Abstract translation: 内酰胺，特别是ε-己内酰胺，是通过氨基腈，特别是6-氨基己腈在气相中水解环化生成的，所述多个绝热固定床反应区依次布置，其中放热的至少一部分热量 在每个连续反应区之间除去反应。 以这种方式进行反应需要较少的反应堆本身资本。 还已经发现，离开这种反应体系的产物可以直接进料到蒸馏装置，而不需要额外的冷却或储存。

    2-bromo-and derivatives of 3-bromo-and 3,3-dibromo-4-oxo-azetidines, processes for the preparation thereof and use thereof
    70.
    发明授权
    2-bromo-and derivatives of 3-bromo-and 3,3-dibromo-4-oxo-azetidines, processes for the preparation thereof and use thereof 失效
    3-溴 - 和3,3-二溴-4-氧代 - 氮杂环丁烷的2-溴衍生物，其制备方法及其用途

    公开(公告)号：US5847119A

    公开(公告)日：1998-12-08

    申请号：US624919

    申请日：1996-03-27

    Applicant: Irena Lukic

    Inventor： Irena Lukic

    IPC: A61K31/395 ,  A61K31/397 ,  A61P31/04 ,  A61P35/00 ,  C07D201/02 ,  C07D205/08

    CPC classification number: A61K31/395 ,  C07D205/08 ,  Y02P20/55

    Abstract: Novel 2-bromo- and 2-nitroxy derivatives of 3-bromo- and 3-dibromo-4-oxo-azetidines, to processes for the preparation thereof and to the use thereof are provided. The azetidines of the present invention have the formula I ##STR1## wherein R.sup.1 is hydrogen or bromine, R.sup.2 is hydrogen or bromine, wherein at least one of R.sup.1 or R.sup.2 is bromine, R.sup.3 is hydrogen; Me.sub.2 --C.dbd.C--COOR.sup.4 wherein R.sup.4 is hydrogen, methyl, benzyl or some other carboxy-protective group, and X is bromine or nitroxy group (--ONO.sub.2). According to the invention 2-bromo- and 2-nitroxy derivatives of 3-bromo- and 3-dibromo-4-oxo-azetidines are prepared by reacting derivatives of protected penicillanic acid 1,1-dioxides with DBN reactant (1,5-diazabicyclo/3.4.0/non-5-ene) and then the obtained DBN salt of sulfinic acid or isolated sulfinic acid is treated with thionyl chloride and, after eliminating thionyl chloride by evaporation, the obtained residue is passed through a silica gel column with methylene chloride or some other solvent as eluant or the obtained residue is dissolved in tetrahydrofuran or some other suitable solvent and treated with tetrabutyl ammonium bromide and after the treatment a derivative of 2-bromo, 3-bromo or 2-bromo-3,3-dibromo-4-oxo-azetidine is isolated, which derivative may be subjected to a reaction with silver nitrate in 2-propanol and, after the treatment of the reaction mixture, derivatives of 2-nitroxy-,3-bromo- or 2-nitroxy-3,3-dibromo-4-oxo-azetidine are isolated. The obtained substances are useful intermediates in the syntheses of beta lactam analogons or as components in formulations having antibacterial, inhibitory, antitumour or antagonistic action.

    Abstract translation: 提供3-溴 - 和3-二溴-4-氧代 - 氮杂环丁烷的新型2-溴 - 和2-硝基氧基衍生物，其制备方法及其用途。 本发明的氮杂环丁烷具有式I其中R 1是氢或溴，R 2是氢或溴，其中R 1或R 2中的至少一个是溴，R 3是氢; Me2-C = C-COOR4，其中R4是氢，甲基，苄基或一些其它羧基保护基，X是溴或硝基氧基（-ONO 2）。 根据本发明，3-溴 - 和3-二溴-4-氧代 - 氮杂环丁烷的2-溴 - 和2-硝基氧基衍生物是通过将受保护的青霉烷酸1,1-二氧化物的衍生物与DBN反应物（1,5- 二氮杂双环/ 3.4.0 /非-5-烯），然后将得到的亚磺酸的DBN盐或分离的亚磺酸用亚硫酰氯处理，通过蒸发除去亚硫酰氯后，将所得残余物通过硅胶柱， 二氯甲烷或一些其它溶剂作为洗脱剂，或将所得残余物溶于四氢呋喃或其它合适的溶剂中，并用四丁基溴化铵处理，处理后，将2-溴，3-溴或2-溴-3,3- 分离出二溴-4-氧代 - 氮杂环丁烷，该衍生物可以与硝酸银在2-丙醇中进行反应，在处理反应混合物后，将2-硝基氧基，3-溴 - 或2-硝基氧基 分离出-3,3-二溴-4-氧代 - 氮杂环丁烷。 获得的物质是合成β-内酰胺类似物或作为具有抗菌，抑制，抗肿瘤或拮抗作用的制剂中的组分的有用中间体。

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