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    Method for production of hydroxylammonium phosphate in the synthesis of caprolactam
    11.
    发明公开
    Method for production of hydroxylammonium phosphate in the synthesis of caprolactam 无效
    Methode zur Herstellung von Hydroxylammoniumphosphat in der Synthese von Kaprolactam

    公开(公告)号：EP1013644A1

    公开(公告)日：2000-06-28

    申请号：EP99125633.0

    申请日：1999-12-22

    Applicant: PRAXAIR TECHNOLOGY, INC.

    Inventor： Echegaray, Diego Fernandez ,  Velloso, Antonio Augusto M. ,  Wagner, Matthew Lincoln

    IPC: C07D201/06 ,  C07D201/10

    CPC classification number: C07D201/06 ,  C07D201/10

    Abstract: A method for production of caprolactam. The method involves:

    (a) reacting air with ammonia gas in an ammonia conversion zone to produce nitric oxide;
    (b) oxidizing at least a portion of the nitric oxide to nitrogen dioxide to produce an NO x -rich process gas stream;
    (c) reactively absorbing the NO x -rich gas stream with phosphoric acid containing solution in an absorption zone to form nitrate ions;
    (d) contacting the nitrate ions with air in a degassing zone to produce a nitrate-rich aqueous process stream;
    (e) reducing the nitrate-rich aqueous stream with hydrogen in the presence of phosphoric acid to produce hydroxylammonium phosphate;
    (f) oximating the hydroxylammonium phosphate with cyclohexanone to produce cyclohexanone oxime; and
    (g) converting the cyclohexanone oxime to caprolactam.
    According to the invention, supplemental oxygen is added downstream of the ammonia conversion zone to increase the quantity and rate of formation of nitrogen dioxide in the NO x -rich process gas stream.

    Abstract translation: 一种生产己内酰胺的方法。 该方法包括：（a）在氨转化区中使空气与氨气反应产生一氧化氮; （b）将至少一部分一氧化氮氧化成二氧化氮以产生富含NO x的工艺气流; （c）在吸收区中用含磷酸溶液反应性吸收富含NO x的气流，形成硝酸根离子; （d）将硝酸根离子与脱气区的空气接触以产生富含硝酸盐的含水工艺物流; （e）在磷酸存在下用氢还原富硝酸盐的水流以产生磷酸羟铵; （f）用环己酮肟化磷酸羟铵，制得环己酮肟; 和（g）将环己酮肟转化为己内酰胺。 根据本发明，在氨转化区的下游添加补充氧以增加富含NOx的工艺气流中二氧化氮的形成量和速率。

    11-(2-PYRROLIDIN-1-YL-ETHOXY)-14,19-DIOXA-5,7,26-TRIAZA-TETRACYCLO[19.3.1.1(2,6).1(8,12)]HEPTACOSA-1(25),2(26),3,5,8,10,12(27),16,21,23-DECAENE CITRATE SALT
    13.
    发明申请
    11-(2-PYRROLIDIN-1-YL-ETHOXY)-14,19-DIOXA-5,7,26-TRIAZA-TETRACYCLO[19.3.1.1(2,6).1(8,12)]HEPTACOSA-1(25),2(26),3,5,8,10,12(27),16,21,23-DECAENE CITRATE SALT 有权
    11-（2-吡咯烷-1-基 - 乙氧基）-14,19-二氧杂环己烯-5,7,26-三唑并[3,4-b] [19.3.1.1（2,6）.1（8,12）] HEPTACOSA-1（ 25），2（26），3,5,8,10,12（27），16,21,23 - 十六烷基硫酸盐

    公开(公告)号：US20110294831A1

    公开(公告)日：2011-12-01

    申请号：US13133297

    申请日：2009-12-09

    Applicant: Brian Dymock ,  Cheng H. Lee ,  Anthony D. William

    Inventor： Brian Dymock ,  Cheng H. Lee ,  Anthony D. William

    IPC: A61K31/395 ,  A61P35/00 ,  C07D498/06

    CPC classification number: C07D498/08 ,  C07B2200/13 ,  C07C55/22 ,  C07D201/10 ,  C07D498/04

    Abstract: The present invention relates to certain salts of a 11-(2-pyrrolidin-1-yl-ethoxy)-14,19-dioxa-5,7,26-triaza-tetracyclo[19.3.1.1(2,6).1(8,12)]heptacosa-1(25),2(26),3,5,8,10,12(27),16,21,23-decaene (Compound I) which have been found to have improved properties. In particular the present invention relates to the citrate salt of this compound. The invention also relates to pharmaceutical compositions containing the citrate salt and methods of use of the citrate salt in the treatment of certain medical conditions.

    Abstract translation: 本发明涉及11-（2-吡咯烷-1-基 - 乙氧基）-14,19-二氧杂-5,7,26-三氮杂 - 四环[19.3.1.1（2,6）.1（ 8,12）]，已被发现具有改善的性能的十七酸-1（25），2（26），3,5,8,10,12（27），16,21,23-十氢烯（化合物I）。 特别地，本发明涉及该化合物的柠檬酸盐。 本发明还涉及含有柠檬酸盐的药物组合物和柠檬酸盐在使用某些医疗条件下的使用方法。

    11-(2-PYRROLIDIN-1-YL-ETHOXY)-14,19-DIOXA-5,7,26-TRIAZA-TETRACYCLO[19.3.1.1(2,6)1(8,12)]HEPTACOSA-1(25),2(26),3,5,8,10,12(27),16,21,23-DECAENE CITRATE SALT
    17.
    发明公开
    11-(2-PYRROLIDIN-1-YL-ETHOXY)-14,19-DIOXA-5,7,26-TRIAZA-TETRACYCLO[19.3.1.1(2,6)1(8,12)]HEPTACOSA-1(25),2(26),3,5,8,10,12(27),16,21,23-DECAENE CITRATE SALT 有权
    11-（2-吡咯烷-1-基 - 乙氧基）-14,19二氧杂5,7,26三氮杂 - 四环[19.3.1.1（2,6）1（8,12）]二十七-1（25 ），2（26），3,5,8,10,12（27），16,21,23-DECAENE CITRATE SALT

    公开(公告)号：EP2376499A1

    公开(公告)日：2011-10-19

    申请号：EP09788621.2

    申请日：2009-12-09

    Applicant: S*BIO Pte Ltd

    Inventor： DYMOCK, Brian ,  LEE, Cheng Hsia Angeline ,  WILLIAM, Anthony Deodaunia

    IPC: C07D498/04 ,  A61K31/519 ,  A61P35/00

    CPC classification number: C07D498/08 ,  C07B2200/13 ,  C07C55/22 ,  C07D201/10 ,  C07D498/04

    Abstract: The present invention relates to certain salts of a 11-(2-pyrrolidin-1-yl-ethoxy)-14,19- dioxa-5,7,26-triaza-tetracyclo[19.3.1.1 (2,6).1 (8, 12)]heptacosa- 1 (25),2(26),3,5,8,10,12(27),16,21,23-decaene (Compound I) which have been found to have improved properties. In particular the present invention relates to the citrate salt of this compound. The invention also relates to pharmaceutical compositions containing the citrate salt and methods of use of the citrate salt in the treatment of certain medical conditions.

    Abstract translation: 本发明涉及11-（2-吡咯烷-1-基 - 乙氧基）-14,19-二氧杂-5,7,26-三氮杂 - 四环[19.3.1.1（2,6）.1（ （25），2（26），3,5,8,10,12（27），16,21,23-十烯（化合物I），其已被发现具有改进的性质。 具体地说，本发明涉及该化合物的柠檬酸盐。 本发明还涉及含有柠檬酸盐的药物组合物和使用该柠檬酸盐治疗某些医学病症的方法。

    11-(2-PYRROLIDIN-1-YL-ETHOXY)-14,19-DIOXA-5,7,26-TRIAZA-TETRACYCLO[19.3.1.1(2,6).1(8,12)]HEPTACOSA-1(25),2(26),3,5,8,10,12(27),16,21,23-DECAENE CITRATE SALT
    19.
    发明申请
    11-(2-PYRROLIDIN-1-YL-ETHOXY)-14,19-DIOXA-5,7,26-TRIAZA-TETRACYCLO[19.3.1.1(2,6).1(8,12)]HEPTACOSA-1(25),2(26),3,5,8,10,12(27),16,21,23-DECAENE CITRATE SALT 审中-公开
    11-（2-吡咯烷-1-基 - 乙氧基）-14,19-二氧杂环己烯-5,7,26-三唑并[3,4-b] [19.3.1.1（2,6）.1（8,12）] HEPTACOSA-1（ 25），2（26），3,5,8,10,12（27），16,21,23 - 十六烷基硫酸盐

    公开(公告)号：US20150322084A1

    公开(公告)日：2015-11-12

    申请号：US14621726

    申请日：2015-02-13

    Applicant: CTI BIOPHARMA CORP.

    Inventor： Brian Dymock ,  Cheng Hsia Angeline Lee ,  Anthony Deodaunia William

    IPC: C07D498/08 ,  C07C55/22

    CPC classification number: C07D498/08 ,  C07B2200/13 ,  C07C55/22 ,  C07D201/10 ,  C07D498/04

    Abstract: The present invention relates to certain salts of a 11-(2-pyrrolidin-1-yl-ethoxy)-14,19-dioxa-5,7,26-triaza-tetracyclo[19.3.1.1(2,6).1(8,12)]heptacosa-1(25),2(26),3,5,8,10,12(27),16,21,23-decaene (Compound I) which have been found to have improved properties. In particular the present invention relates to the citrate salt of this compound. The invention also relates to pharmaceutical compositions containing the citrate salt and methods of use of the citrate salt in the treatment of certain medical conditions.

    Abstract translation: 本发明涉及11-（2-吡咯烷-1-基 - 乙氧基）-14,19-二氧杂-5,7,26-三氮杂 - 四环[19.3.1.1（2,6）.1（ 8,12）]，已被发现具有改善的性能的十七酸-1（25），2（26），3,5,8,10,12（27），16,21,23-十氢烯（化合物I）。 特别地，本发明涉及该化合物的柠檬酸盐。 本发明还涉及含有柠檬酸盐的药物组合物和柠檬酸盐在使用某些医疗条件下的使用方法。

    Method for production of hydroxylamine sulfate in the conventional process for the synthesis of caprolactam
    20.
    发明授权
    Method for production of hydroxylamine sulfate in the conventional process for the synthesis of caprolactam 有权
    用于合成己内酰胺的常规方法生产硫酸羟胺的方法

    公开(公告)号：US06469163B1

    公开(公告)日：2002-10-22

    申请号：US09221209

    申请日：1998-12-24

    Applicant: Diego Fernandez Echegaray ,  Antonio Augusto M. Velloso ,  Matthew Lincoln Wagner

    Inventor： Diego Fernandez Echegaray ,  Antonio Augusto M. Velloso ,  Matthew Lincoln Wagner

    IPC: C07D20104

    CPC classification number: C07D201/06 ,  C07D201/10

    Abstract: An improvement in the conventional process for the production of caprolactam. The process involves: (a) reacting air with ammonia gas in an ammonia conversion zone to produce nitric oxide; (b) oxidizing a portion of the nitric oxide to nitrogen dioxide to produce an NOx-rich process gas stream; (c) reacting the NOx-rich stream with ammonium carbonate in a nitriting zone to produce ammonium nitrite; (d) reducing the ammonium nitrite to hydroxylamine diammonium sulfate; (e) hydrolyzing the hydroxylamine diammonium sulfate to hydroxylamine sulfate; (f) oximating the hydroxylamine sulfate with cyclohexanone to produce cyclohexanone oxime; and (g) converting the cyclohexanone oxime to caprolactam. The process is improved by adding supplemental oxygen downstream of the ammonia conversion zone to increase the quantity and rate of formation of nitrogen dioxide in the NOx-rich process gas stream.

    Abstract translation: 制备己内酰胺的常规方法的改进。 该方法包括：（a）在氨转化区中使空气与氨气反应以产生一氧化氮;（b）将一部分氧化氮氧化成二氧化氮以产生富含NO x的工艺气流;（c）使 在氮化区中用碳酸铵生成富含NO x的物流以产生亚硝酸铵;（d）将亚硝酸铵还原为羟胺二硫酸铵;（e）将羟胺二硫酸铵水解成硫酸羟胺;（f）用环己酮将硫酸羟胺酸化 生产环己酮肟; 并且（g）将环己酮肟转化为己内酰胺。通过在氨转化区下游加入补充氧以提高富氮过程气流中二氧化氮形成的数量和速率，从而提高了工艺。

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