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1. 发明申请

US20110065913A1 PROCESS FOR PRODUCING LAUROLACTAM 有权
标题翻译：生产乳酸菌的方法
公开(公告)号：US20110065913A1
公开(公告)日：2011-03-17
申请号：US12993451
申请日：2009-05-19
申请人： Junichi Kugimoto , Nobuhiro Ii , Takashi Doi , Satoru Fujitsu , Tadashi Gotou , Hideo Shimomura , Ryouta Yasumatsu , Joji Kawai
发明人： Junichi Kugimoto , Nobuhiro Ii , Takashi Doi , Satoru Fujitsu , Tadashi Gotou , Hideo Shimomura , Ryouta Yasumatsu , Joji Kawai
IPC分类号： C07D225/02
CPC分类号： C07D201/04 , C07D225/02
摘要： The present invention relates to a process for producing laurolactam from cyclododecanone oxime by liquid-phase rearrangement reaction using trichlorotriazine as a rearrangement catalyst. The present invention can provide a process which can solve the problem of termination of the reaction at a certain conversion, can prevent an inactive precipitate generated from trichlorotriazine from precipitating in the course of the reaction process, and can remove an inactive precipitate, an active intermediate and a residual catalyst.
摘要翻译：本发明涉及使用三氯三嗪作为重排催化剂通过液相重排反应从环十二酮肟生产十二内酰胺的方法。本发明可以提供能够解决在一定转化时终止反应的问题的方法，可以防止三氯三嗪在反应过程中产生的不活泼的沉淀物沉淀，并且可以除去无活性的沉淀物，活性中间体和残留催化剂。

2. 发明授权

US08309714B2 Process for producing laurolactam 有权
标题翻译：生产月桂内酰胺的方法
公开(公告)号：US08309714B2
公开(公告)日：2012-11-13
申请号：US12744675
申请日：2008-11-19
申请人： Junichi Kugimoto , Joji Kawai , Hideo Shimomura , Ryouta Yasumatsu , Nobuhiro Ii
发明人： Junichi Kugimoto , Joji Kawai , Hideo Shimomura , Ryouta Yasumatsu , Nobuhiro Ii
IPC分类号： C07D201/04 , C07D225/02
CPC分类号： C07D201/04 , C07D225/02 , Y02P20/582
摘要： Provided is a process for efficiently producing laurolactam by simple steps from cyclododecanone and hydroxylamine. This production process comprises the steps of: (a) reacting cyclododecanone with hydroxylamine in an aqueous solution in the presence of an oxime-formation solvent to produce cyclododecanone oxime; (b) separating the reaction mixture obtained after the oxime-forming step into an oil and an aqueous phases and collecting a solution of cyclododecanone oxime of the oil phase; (c) removing a part or all of the oxime-formation solvent and dissolved water from the solution of cyclododecanone oxime which is collected as an oil phase in the oil/aqueous phase separation step, whereby preparing a solution containing a rearrangement solvent to be used in a rearrangement reaction in a later step and the cyclododecanone oxime; (d) producing laurolactam from cyclododecanone oxime by rearrangement reaction using an aromatic-ring containing compound as a rearrangement catalyst; and (e) separating and removing the rearrangement solvent and the rearrangement catalyst from the reaction mixture after the rearrangement step, and purifying the laurolactam.
摘要翻译：提供一种通过简单的步骤从环十二酮和羟胺有效地生产十二内酰胺的方法。该制备方法包括以下步骤：（a）在肟形成溶剂存在下，使环十二酮与羟胺在水溶液中反应，生成环十二烷酮肟; （b）将在肟形成步骤后获得的反应混合物分离成油相和水相，并收集油相的环十二烷酮肟溶液; （c）从油/水相分离步骤中以油相收集的环十二烷酮肟溶液中除去部分或全部肟形成溶剂和溶解的水，由此制备含有使用的重排溶剂的溶液在后续步骤中的重排反应和环十二酮肟; （d）使用含芳环的化合物作为重排催化剂，通过重排反应从环十二酮肟生产月桂内酰胺; 和（e）在重排步骤之后从反应混合物中分离和除去重排溶剂和重排催化剂，并纯化月桂内酰胺。

3. 发明授权

US08338589B2 Process for producing laurolactam 有权
标题翻译：生产月桂内酰胺的方法
公开(公告)号：US08338589B2
公开(公告)日：2012-12-25
申请号：US12993451
申请日：2009-05-19
申请人： Junichi Kugimoto , Nobuhiro Ii , Takashi Doi , Satoru Fujitsu , Tadashi Gotou , Hideo Shimomura , Ryouta Yasumatsu , Joji Kawai
发明人： Junichi Kugimoto , Nobuhiro Ii , Takashi Doi , Satoru Fujitsu , Tadashi Gotou , Hideo Shimomura , Ryouta Yasumatsu , Joji Kawai
IPC分类号： C07D201/04 , C07D225/02
CPC分类号： C07D201/04 , C07D225/02
摘要： The present invention relates to a process for producing laurolactam from cyclododecanone oxime by liquid-phase rearrangement reaction using trichlorotriazine as a rearrangement catalyst. The present invention can provide a process which can solve the problem of termination of the reaction at a certain conversion, can prevent an inactive precipitate generated from trichlorotriazine from precipitating in the course of the reaction process, and can remove an inactive precipitate, an active intermediate and a residual catalyst.
摘要翻译：本发明涉及使用三氯三嗪作为重排催化剂通过液相重排反应从环十二酮肟生产十二内酰胺的方法。本发明可以提供能够解决在一定转化时终止反应的问题的方法，可以防止三氯三嗪在反应过程中产生的不活泼的沉淀物沉淀，并且可以除去无活性的沉淀物，活性中间体和残留催化剂。

4. 发明申请

US20100267944A1 PROCESS FOR PRODUCING LAUROLACTAM 有权
标题翻译：生产乳酸菌的方法
公开(公告)号：US20100267944A1
公开(公告)日：2010-10-21
申请号：US12744675
申请日：2008-11-19
申请人： Junichi Kugimoto , Joji Kawai , Hideo Shimomura , Ryouta Yasumatsu , Nobuhiro II
发明人： Junichi Kugimoto , Joji Kawai , Hideo Shimomura , Ryouta Yasumatsu , Nobuhiro II
IPC分类号： C07D225/02
CPC分类号： C07D201/04 , C07D225/02 , Y02P20/582
摘要： Provided is a process for efficiently producing laurolactam by simple steps from cyclododecanone and hydroxylamine. This production process comprises the steps of: (a) reacting cyclododecanone with hydroxylamine in an aqueous solution in the presence of an oxime-formation solvent to produce cyclododecanone oxime; (b) separating the reaction mixture obtained after the oxime-forming step into an oil and an aqueous phases and collecting a solution of cyclododecanone oxime of the oil phase; (c) removing a part or all of the oxime-formation solvent and dissolved water from the solution of cyclododecanone oxime which is collected as an oil phase in the oil/aqueous phase separation step, whereby preparing a solution containing a rearrangement solvent to be used in a rearrangement reaction in a later step and the cyclododecanone oxime; (d) producing laurolactam from cyclododecanone oxime by rearrangement reaction using an aromatic-ring containing compound as a rearrangement catalyst; and (e) separating and removing the rearrangement solvent and the rearrangement catalyst from the reaction mixture after the rearrangement step, and purifying the laurolactam.
摘要翻译：提供一种通过简单的步骤从环十二酮和羟胺有效地生产十二内酰胺的方法。该制备方法包括以下步骤：（a）在肟形成溶剂存在下，使环十二酮与羟胺在水溶液中反应，生成环十二酮肟; （b）将在肟形成步骤后获得的反应混合物分离成油相和水相，并收集油相的环十二烷酮肟溶液; （c）从油/水相分离步骤中以油相收集的环十二酮肟溶液中除去部分或全部肟形成溶剂和溶解的水，由此制备含有使用的重排溶剂的溶液在后续步骤中的重排反应和环十二酮肟; （d）使用含芳环的化合物作为重排催化剂，通过重排反应从环十二酮肟生产月桂内酰胺; 和（e）在重排步骤之后从反应混合物中分离和除去重排溶剂和重排催化剂，并纯化月桂内酰胺。

5. 发明授权

US08624021B2 Compound and process for producing amide compound therewith 有权
标题翻译：用于生产酰胺化合物的化合物和方法
公开(公告)号：US08624021B2
公开(公告)日：2014-01-07
申请号：US13497687
申请日：2010-09-24
申请人： Tsunemi Sugimoto , Mitsuru Kishishita , Junichi Kugimoto , Kazunori Kurosawa , Hideo Shimomura , Ryouta Yasumatsu
发明人： Tsunemi Sugimoto , Mitsuru Kishishita , Junichi Kugimoto , Kazunori Kurosawa , Hideo Shimomura , Ryouta Yasumatsu
IPC分类号： C07D225/02 , C07D201/04
CPC分类号： C07D201/04 , C07D225/02
摘要： The present invention provides novel cyclododecanone-O-azacyclotridecen-2-yloxime and cyclododecanone-O-azacyclotridecen-2-yloxime hydrochloride. The invention also provides a process for producing an amide compound wherein cyclododecanone-O-azacyclotridecen-2-yloxime, hydrogen chloride and/or Lewis acid or cyclododecanone-O-azacyclotridecen-2-yloxime hydrochloride are used as a rearrangement catalyst and/or a reaction starting material in a reaction step.
摘要翻译：本发明提供了新的环十二烷酮-O-氮杂环十二烯-2-基肟和环十二酮-O-氮杂环十二烯-2-基肟酸盐酸盐。本发明还提供一种制备酰胺化合物的方法，其中使用环十二酮-O-氮杂环十二碳-2-肟，氯化氢和/或路易斯酸或环十二烷酮-O-氮杂环十二烯-2-基肟酸盐酸盐作为重排催化剂和/或反应步骤中的反应原料。

6. 发明申请

US20130005961A1 NOVEL COMPOUND AND PROCESS FOR PRODUCING AMIDE COMPOUND THEREWITH 有权
标题翻译：新型化合物及其生产方法
公开(公告)号：US20130005961A1
公开(公告)日：2013-01-03
申请号：US13497687
申请日：2010-09-24
申请人： Tsunemi Sugimoto , Mitsuru Kishishita , Junichi Kugimoto , Kazunori Kurosawa , Hideo Shimomura , Ryouta Yasumatsu
发明人： Tsunemi Sugimoto , Mitsuru Kishishita , Junichi Kugimoto , Kazunori Kurosawa , Hideo Shimomura , Ryouta Yasumatsu
IPC分类号： C07D225/02
CPC分类号： C07D201/04 , C07D225/02
摘要： The present invention provides novel cyclododecanone-O-azacyclotridecen-2-yloxime and cyclododecanone-O-azacyclotridecen-2-yloxime hydrochloride. The invention also provides a process for producing an amide compound wherein cyclododecanone-O-azacyclotridecen-2-yloxime, hydrogen chloride and/or Lewis acid or cyclododecanone-O-azacyclotridecen-2-yloxime hydrochloride are used as a rearrangement catalyst and/or a reaction starting material in a reaction step.
摘要翻译：本发明提供新的环十二烷酮-O-氮杂环十二烷-2-基肟和环十二烷酮-O-氮杂环十二烯-2-基肟酸盐酸盐。本发明还提供一种制备酰胺化合物的方法，其中使用环十二酮-O-氮杂环十二碳-2-肟，氯化氢和/或路易斯酸或环十二烷酮-O-氮杂环十二烯-2-基肟酸盐酸盐作为重排催化剂和/或反应步骤中的反应原料。

7. 发明授权

US08163899B2 Process for producing laurolactam 有权
标题翻译：生产月桂内酰胺的方法
公开(公告)号：US08163899B2
公开(公告)日：2012-04-24
申请号：US12526494
申请日：2008-02-08
申请人： Kazuaki Ishihara , Junichi Kugimoto , Joji Kawai
发明人： Kazuaki Ishihara , Junichi Kugimoto , Joji Kawai
IPC分类号： C07D201/04
CPC分类号： C07D201/04 , C07D225/02 , Y02P20/582
摘要： Disclosed is a method for producing laurolactam from cyclododecanone and hydroxylamine in a simple process and with high efficiency. The method comprises the following steps (a) to (e): (a) reacting cyclododecanone with hydroxylamine in an aqueous solution in the presence of an excess amount of cyclododecanone or a solvent to produce cyclododecanone oxime; (b) separating the reaction mixture obtained after the oxime-forming step into an oil and an aqueous phases and collecting a solution of cyclododecanone oxime of the oil phase as; (c) removing dissolved water from the solution of cyclododecanone oxime which is collected as an oily phase in the oil/aqueous phase separation step; (d) producing laurolactam from cyclododecanone oxime by rearrangement reaction using an aromatic-ring containing compound as a rearrangement catalyst; and (e) separating the produced laurolactam from the reaction mixture after the rearrangement step and purifying the laurolactam.
摘要翻译：公开了一种以简单的工艺和高效率从环十二酮和羟胺制备月桂内酰胺的方法。该方法包括以下步骤（a）至（e）：（a）在过量的环十二烷酮或溶剂的存在下，使环十二酮与羟胺在水溶液中反应，生成环十二酮肟; （b）将在肟形成步骤后获得的反应混合物分离成油和水相，并收集油相的环十二酮肟溶液; （c）从在油/水相分离步骤中以油相收集的环十二酮肟溶液中除去溶解的水; （d）使用含芳环的化合物作为重排催化剂，通过重排反应从环十二酮肟生产月桂内酰胺; 和（e）在重排步骤之后将所生产的月桂内酰胺与反应混合物分离并纯化十二内酰胺。

8. 发明申请

US20130005960A1 METHOD FOR PRODUCING AMIDE COMPOUND 有权
标题翻译：生产酰胺化合物的方法
公开(公告)号：US20130005960A1
公开(公告)日：2013-01-03
申请号：US13635092
申请日：2011-03-15
申请人： Junichi Kugimoto , Joji Kawai , Kazuo Yamato , Masahide Okada , Tsunemi Sugimoto , Hiroshi Matsumoto
发明人： Junichi Kugimoto , Joji Kawai , Kazuo Yamato , Masahide Okada , Tsunemi Sugimoto , Hiroshi Matsumoto
IPC分类号： C07D225/02
CPC分类号： C07D201/06 , C07D201/04 , C07D225/02
摘要： The present invention relates to a method for producing a high purity, high quality amide compound, particularly, lactam. A first embodiment of the present invention is characterized in that an amount of each of a halide, an aldehyde compound, an alcohol compound and a nitrile compound contained in a solution recycled into an oxime-forming step is controlled to an amount of 0.4 mol % or less based on the ketone as a starting material. A second embodiment of the present invention is characterized in that one or more compounds selected from the group consisting of a ketone, an oxime and an amide compound are purified by hydrogenation and/or crystallization for eliminating impurities containing a double bond. A third embodiment of the present invention is characterized in that a content of impurities having a cyclic bridge structure is controlled by using a cycloalkanone purified by recrystallization.
摘要翻译：本发明涉及一种生产高纯度，优质酰胺化合物，特别是内酰胺的方法。本发明的第一实施方案的特征在于，将再循环到肟形成步骤的溶液中所含的卤化物，醛化合物，醇化合物和腈化合物中的每一种的量控制为0.4mol％基于酮作为原料。本发明的第二个实施方案的特征在于，通过氢化和/或结晶纯化一种或多种选自酮，肟和酰胺化合物的化合物，以消除含有双键的杂质。本发明的第三实施方案的特征在于通过使用通过重结晶纯化的环烷酮来控制具有环状桥结构的杂质的含量。

9. 发明授权

US08816069B2 Method for producing amide compound 有权
标题翻译：酰胺化合物的制备方法
公开(公告)号：US08816069B2
公开(公告)日：2014-08-26
申请号：US13635092
申请日：2011-03-15
申请人： Junichi Kugimoto , Joji Kawai , Hiroshi Matsumoto
发明人： Junichi Kugimoto , Joji Kawai , Hiroshi Matsumoto
IPC分类号： C07D225/02 , C07D201/04 , C07D201/06
CPC分类号： C07D201/06 , C07D201/04 , C07D225/02
摘要： The present invention relates to a method for producing a high purity, high quality amide compound, particularly, lactam. A first embodiment of the present invention is characterized in that an amount of each of a halide, an aldehyde compound, an alcohol compound and a nitrile compound contained in a solution recycled into an oxime-forming step is controlled to an amount of 0.4 mol % or less based on the ketone as a starting material. A second embodiment of the present invention is characterized in that one or more compounds selected from the group consisting of a ketone, an oxime and an amide compound are purified by hydrogenation and/or crystallization for eliminating impurities containing a double bond. A third embodiment of the present invention is characterized in that a content of impurities having a cyclic bridge structure is controlled by using a cycloalkanone purified by recrystallization.
摘要翻译：本发明涉及一种生产高纯度，优质酰胺化合物，特别是内酰胺的方法。本发明的第一实施方案的特征在于，将再循环到肟形成步骤的溶液中所含的卤化物，醛化合物，醇化合物和腈化合物中的每一种的量控制为0.4mol％基于酮作为原料。本发明的第二个实施方案的特征在于，通过氢化和/或结晶纯化一种或多种选自酮，肟和酰胺化合物的化合物，以消除含有双键的杂质。本发明的第三实施方案的特征在于通过使用通过重结晶纯化的环烷酮来控制具有环状桥结构的杂质的含量。

10. 发明申请

US20100324283A1 PROCESS FOR PRODUCING LAUROLACTAM 有权
标题翻译：生产乳酸菌的方法
公开(公告)号：US20100324283A1
公开(公告)日：2010-12-23
申请号：US12526494
申请日：2008-02-08
申请人： Kazuaki Ishihara , Junichi Kugimoto , Joji Kawai
发明人： Kazuaki Ishihara , Junichi Kugimoto , Joji Kawai
IPC分类号： C07D225/02
CPC分类号： C07D201/04 , C07D225/02 , Y02P20/582
摘要： Disclosed is a method for producing laurolactam from cyclododecanone and hydroxylamine in a simple process and with high efficiency. The method comprises the following steps (a) to (e): (a) reacting cyclododecanone with hydroxylamine in an aqueous solution in the presence of an excess amount of cyclododecanone or a solvent to produce cyclododecanone oxime; (b) separating the reaction mixture obtained after the oxime-forming step into an oil and an aqueous phases and collecting a solution of cyclododecanone oxime of the oil phase as; (c) removing dissolved water from the solution of cyclododecanone oxime which is collected as an oily phase in the oil/aqueous phase separation step; (d) producing laurolactam from cyclododecanone oxime by rearrangement reaction using an aromatic-ring containing compound as a rearrangement catalyst; and (e) separating the produced laurolactam from the reaction mixture after the rearrangement step and purifying the laurolactam.
摘要翻译：公开了一种以简单的工艺和高效率从环十二酮和羟胺制备月桂内酰胺的方法。该方法包括以下步骤（a）至（e）：（a）在过量的环十二烷酮或溶剂存在下，使环十二酮与羟胺在水溶液中反应，生成环十二酮肟; （b）将在肟形成步骤后获得的反应混合物分离成油和水相，并收集油相的环十二酮肟溶液; （c）从在油/水相分离步骤中以油相收集的环十二酮肟溶液中除去溶解的水; （d）使用含芳环的化合物作为重排催化剂，通过重排反应从环十二酮肟生产月桂内酰胺; 和（e）在重排步骤之后将所生产的月桂内酰胺与反应混合物分离并纯化十二内酰胺。

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