公开(公告)号：US06344557B1

公开(公告)日：2002-02-05

申请号：US09674164

申请日：2000-10-27

申请人： Masami Fukao ,  Kan Takamine ,  Tomokazu Nakamura

发明人： Masami Fukao ,  Kan Takamine ,  Tomokazu Nakamura

IPC分类号： C07D20116

CPC分类号： C07D201/04

摘要： The present invention provides a method for producing &egr;-caprolactam which comprises the step of treating, with water, a reaction product containing 1-aza-2-alkoxy-1-cycloheptene, which is obtained by gas phase Beckmann rearrangement reaction of cyclohexanone oxime using a solid catalyst in the presence of alcohol, to eliminate the 1-aza-2-alkoxy-1-cycloheptene. The resulting &egr;-caprolactam usually has a 1-aza-2-alkoxy-1-cycloheptene content of 100 ppm or less, preferably 25 ppm or less, more preferably 10 ppm or less and, therefore, has low free basicity and good qualities.

摘要翻译： 本发明提供一种ε-己内酰胺的制造方法，其包括用水处理含有1-氮杂-2-烷氧基-1-环庚烯的反应产物的步骤，该反应产物是通过环己酮肟的气相贝克曼重排反应得到的，使用 在醇存在下的固体催化剂，以除去1-氮杂-2-烷氧基-1-环庚烯。 所得的ε-己内酰胺通常具有100ppm以下的1-氮杂-2-烷氧基-1-环庚烯含量，优选为25ppm以下，更优选为10ppm以下，因此具有低的游离碱度和良好的品质。

公开(公告)号：US06252068B1

公开(公告)日：2001-06-26

申请号：US09472172

申请日：1999-12-27

申请人： Masami Fukao ,  Kan Takamine

发明人： Masami Fukao ,  Kan Takamine

IPC分类号： C07D20116

CPC分类号： C07D201/16

摘要： A high purity &egr;-caprolactam is prepared by crystallizing an &egr;-caprolactam from a hydrocarbon solution containing a crude &egr;-caprolactam, and allowing the crystallized &egr;-caprolactam in contact with hydrogen in the presence of a hydrogenation catalyst. This process can effectively remove impurities from a crude &egr;-caprolactam, which is obtained by subjecting cyclohexanone oxime to the Beckmann rearrangement, and provide a high purity &egr;-caprolactam.

摘要翻译： 通过从含有ε-己内酰胺的烃溶液中使ε-己内酰胺结晶，并在氢化催化剂的存在下使结晶的ε-己内酰胺与氢气接触来制备高纯度ε-己内酰胺。 该方法可以有效地除去通过使环己酮肟进行贝克曼重排而得到的粗ε-己内酰胺中的杂质，并提供高纯度ε-己内酰胺。

公开(公告)号：US5442114A

公开(公告)日：1995-08-15

申请号：US182460

申请日：1994-01-18

申请人： Kan Takamine ,  Michio Yamato ,  Akira Murakami ,  Tooru Tokumaru ,  Yoshinori Nakayama ,  Motoo Hazama

发明人： Kan Takamine ,  Michio Yamato ,  Akira Murakami ,  Tooru Tokumaru ,  Yoshinori Nakayama ,  Motoo Hazama

IPC分类号： C07C231/02 ,  C07C235/24

CPC分类号： C07C231/02 ,  C07C235/24

摘要： There is disclosed a process for producing an aromatic amide compound of the general formula (4), including the steps of subjecting an o-nitrophenol compound of the general formula (1) to catalytic reduction in acetone or an aromatic hydrocarbon solvent under the presence of a nickel catalyst to give an o-aminophenol compound of the general formula (2); and (b) subjecting the o-aminophenol compound of the general formula (2) to condensation with an acid chloride compound having a sulfur content of 0.5% or less, based on the weight of the acid chloride compound, of the general formula (3) in acetone or an aromatic hydrocarbon solvent under an atmosphere of an inert gas having an oxygen concentration of 1% or less. The acid chloride compound having a sulfur content of 0.5% or less, based on the weight of the acid chloride compound, of the general formula (3) may be obtained by allowing a carboxylic acid compound of the general formula (5) to react with thionyl chloride and by concentrating the reaction mixture. Also disclosed is another process for producing an aromatic amide compound of the general formula (4), including the step of subjecting an o-aminophenol hydrochloride salt of the general formula (6) to condensation with an acid chloride compound having a sulfur content of 0.8% or less, based on the weight of the acid chloride compound, of the general formula (3) in an inert solvent.

摘要翻译： 公开了通式（4）的芳香族酰胺化合物的制造方法，包括以下步骤：将通式（1）的邻硝基苯酚化合物在丙酮或芳族烃溶剂中进行催化还原， 镍催化剂，得到通式（2）的邻氨基苯酚化合物; 和（b）将通式（2）的邻氨基苯酚化合物与基于酰基氯化合物的重量的硫含量为0.5％以下的酰基氯化合物进行缩合，通式（3） ）在丙酮或芳烃溶剂中，在氧浓度为1％以下的惰性气体气氛下进行。 通式（3）的酰基氯化合物的硫含量为0.5％以下的酰氯化合物可以通过使通式（5）的羧酸化合物与 亚硫酰氯，并浓缩反应混合物。 还公开了制备通式（4）的芳族酰胺化合物的另一种方法，包括使通式（6）的邻氨基苯酚盐酸盐与硫含量为0.8的酰氯化合物缩合的步骤 ％以下，基于酰基氯化合物的重量，在惰性溶剂中。