公开(公告)号：JP2001122808A

公开(公告)日：2001-05-08

申请号：JP2000240217

申请日：2000-08-08

Applicant: DAICEL CHEM

Inventor： WATANABE HITOSHI ,  HIRAI NARIHISA ,  SHIMAMURA MASAMI ,  MIURA HIROYUKI

IPC: C07C27/12 ,  C07B61/00 ,  C07C45/36 ,  C07C47/542 ,  C07C51/265 ,  C07C63/04

Abstract: PROBLEM TO BE SOLVED: To produce benzaldehydes and/or benzoic acids with a good production efficiency while suppressing side reactions without using a catalyst having great corrosiveness. SOLUTION: This method for producing an aromatic compound comprises (A) an oxidation step for bringing toluenes which may have a substituent group in the benzene ring into contact with molecular oxygen in the presence of an N-substituted cyclic imide-based catalyst and oxidizing the toluenes, (B) a first extraction step for adding water to the reactional mixture and carrying out the extraction, (C) a first neutralizing step for adding an aqueous solution of an alkali to an organic layer obtained in the first extraction step, neutralizing the organic layer and separating the liquids and (D) at least one step selected from (D1) a benzaldehydes recovering step for recovering the benzaldehydes produced from the organic layer prepared in the first neutralizing step by the reaction and (D2) a benzoic acids recovering step for adding an acid to the aqueous layer obtained by the first neutralizing step, acidifying the aqueous layer and recovering the benzoic acids produced by the reaction.

公开(公告)号：JP2002308820A

公开(公告)日：2002-10-23

申请号：JP2001106386

申请日：2001-04-04

Applicant: DAICEL CHEM

Inventor： WATANABE HITOSHI ,  KUWANA AKIHIRO ,  SHIMAMURA MASAMI

IPC: C07D209/48 ,  C07B61/00 ,  C07C51/265 ,  C07C51/43 ,  C07C51/47 ,  C07C55/14 ,  C07C63/04 ,  C07C63/24 ,  C07C63/26 ,  C07C63/313

Abstract: PROBLEM TO BE SOLVED: To provide a method capable of efficiently separating an oxidizing catalyst and a high purity reaction product (aromatic carboxylic acid or the like) by simple operation. SOLUTION: A substrate and oxygen are brought into contact with each other in the presence of the oxidizing catalyst such as N-hydroxyphthalimide, N-acetoxyphthalimide or the like and a solvent is used to crystallize the reaction product by cooling crystallization or a crystallzing solvent and the oxidizing catalyst is distributed to a solvent phase. The reaction product may be concentrated prior to the crystallization of the reaction product. This method uses a 1-4C alkanecarboxylic acid, 1-10C alkyl alcohol or a water-containing solvent as the crystallizing solvent and the reaction product is useful for separating 6 or more C aliphatic carboxylic acid or aromatic carboxylic acid and the oxidizing catalyst.

公开(公告)号：JP2004123561A

公开(公告)日：2004-04-22

申请号：JP2002286364

申请日：2002-09-30

Applicant: Daicel Chem Ind Ltd ,  ダイセル化学工業株式会社

Inventor： KITAYAMA KENJI ,  SHIMAMURA MASAMI

IPC: C07C45/82 ,  C07B61/00 ,  C07C45/34 ,  C07C49/653 ,  C11B9/00

CPC classification number: Y02P20/55

Abstract: PROBLEM TO BE SOLVED: To provide a method for efficiently manufacturing nootkatone of high qualities from valencene. SOLUTION: In the method for manufacturing the nootkatone, the valencene is reacted with oxygen in the presence of a catalyst comprising an imide compound bearing a cyclic imide skeleton represented by formula (I) [wherein (n) is 0 or 1; and X is oxygen atom or an OR group (wherein R is hydrogen atom or a protecting group of hydroxy group)]. The method comprises (A) a heating treatment step for decomposing a reaction by-product by heating an oxidation reaction mixture, (B) an extraction step for extracting the nootkatone from the mixture after the heat treatment, (C) a basic solution washing step for washing, with a basic solution, the mixture containing the nootkatone after the extraction treatment, and (D) a distillation step for distilling the mixture containing the nootkatone after the extraction treatment to recover the nootkatone. COPYRIGHT: (C)2004,JPO

Abstract translation: 要解决的问题：提供一种有效地制备从戊烯得到高品质的诺卡酮的方法。 解决方案：在制备诺塔卡酮的方法中，在含有式（I）表示的环状酰亚胺骨架的酰亚胺化合物的催化剂存在下，使戊烯与氧反应[其中（n）为0或1; X为氧原子或OR基（其中R为氢原子或羟基保护基）]。 该方法包括：（A）通过加热氧化反应混合物来分解反应副产物的加热处理步骤，（B）从热处理后的混合物中提取诺卡可酮的提取步骤，（C）碱性溶液洗涤步骤 用碱性溶液洗涤在提取处理后含有诺卡酮的混合物，和（D）蒸馏步骤，用于在提取处理后蒸馏含有诺塔卡酮的混合物以回收诺卡可酮。 版权所有（C）2004，JPO

公开(公告)号：JP2002320861A

公开(公告)日：2002-11-05

申请号：JP2001132078

申请日：2001-04-27

Applicant: DAICEL CHEM

Inventor： WATANABE HITOSHI ,  SHIMAMURA MASAMI

IPC: C07D209/48 ,  B01J31/22 ,  B01J31/40 ,  B01J38/00

Abstract: PROBLEM TO BE SOLVED: To provide a method to separate imide compounds and a metal catalyst from a mixture containing the imide compounds and the metal catalyst. SOLUTION: The imide compounds and the metal catalyst are separated from a mixture composed of the imide compounds (N-acetoxyphthalimide, N- hydroxyphthalimide or the like) and the metal catalyst (water-soluble promoter or the like) by using a specified aqueous solvent (e.g. water) and a nonaqueous soluble solvent (alcohols, nitriles, hydrocarbons or a mixture solvent of these).

公开(公告)号：JP2002003470A

公开(公告)日：2002-01-09

申请号：JP2000190224

申请日：2000-06-23

Applicant: DAICEL CHEM

Inventor： SHIMAMURA MASAMI ,  WATANABE HITOSHI

IPC: C07D223/10 ,  C07B61/00 ,  C07D201/02 ,  C07D201/16

Abstract: PROBLEM TO BE SOLVED: To efficiently obtain a lactam from a corresponding cycloalkane. SOLUTION: This method for producing a lactam comprises reacting a cycloalkane with a nitrogen oxide in the presence of an N-substituted cyclic imide-based catalyst and a halogen or Beckmann rearrangement catalyst to produce a corresponding lactam and is composed of (A) a reaction process for bringing the cycloalkane into contact with the nitrogen oxide in the presence of the catalyst and (B) a lactam recovery process for recovering the lactam from the reaction mixture by at least one operation selected from crystallization, distillation and extraction. Before the lactam recovery process (B), (C) a concentration process for concentrating the reaction mixture and distilling away a reaction solvent and/or the unreacted cycloalkane, (D) a base treatment process for treating the reaction mixture with a base, (E) a water extraction process for subjecting the reaction mixture to an extraction operation using water and an organic solvent and transferring the lactam to a water layer side, etc., may be provided.

公开(公告)号：JP2001335549A

公开(公告)日：2001-12-04

申请号：JP2000160367

申请日：2000-05-30

Applicant: DAICEL CHEM

Inventor： SHIMAMURA MASAMI ,  WATANABE HITOSHI

IPC: B01J31/02 ,  B01J38/00 ,  C07B61/00 ,  C07C249/06 ,  C07C249/14 ,  C07C251/44

Abstract: PROBLEM TO BE SOLVED: To provide a method of efficiently producing a cycloalkanone oxime in high yield. SOLUTION: A cycloalkanone oxime is efficiently produced through the following steps: The step (A) where a cycloalkane is reacted with nitrogen oxides in the presence of a specific imide (the reactor 1), the step (B) where the non-crystallized component including nitrocycloalkane and the crystallized component including the catalyst and the cychloalkanone oxime are separated from the reaction mixture (the crystallization tank 3 and the filter 4), and then the catalyst is separated from the crystallization component (the repulping tank 5 and the filter 6) while the cycloalkanone oxime is separated from the filtrate (distillation columns 7, 8). The cycloalkanone oxime is produced with high efficiency by those steps. In another embodiment, the reaction mixture from the reactor 1 may be concentrated in the concentration step (C) (the concentrator 2).

公开(公告)号：JP2001288122A

公开(公告)日：2001-10-16

申请号：JP2000102796

申请日：2000-04-04

Applicant: DAICEL CHEM

Inventor： SHIMAMURA MASAMI ,  HIRAI NARIHISA ,  WATANABE HITOSHI

IPC: B01J31/40 ,  B01J38/00 ,  C07B63/00 ,  C07C29/86 ,  C07C33/20 ,  C07C35/08 ,  C07C45/80 ,  C07C47/542 ,  C07C49/385 ,  C07C49/587 ,  C07C49/643 ,  C07C49/76 ,  C07C49/786 ,  C07C63/00 ,  C07C63/04

Abstract: PROBLEM TO BE SOLVED: To provide a method for separating a reaction product from a catalyst, in which the reaction product from the catalyst and/or the changed catalyst can be separated, by simple operations where an imide compound such as N- hydroxyphthalimide is used as the catalyst and a hydrocarbon or the like as one of solvents. SOLUTION: This method for separating the reaction product from the catalyst and/or the changed catalyst in a reaction mixture obtained by a reaction in the presence of an imide compound catalyst represented by the general formula (1) (R1 and R2 are each H, an alkyl or the like, provided that R1 and R2 may be bound to each other to form a double bond or an aromatic or non- aromatic ring; X is oxygen atom hydroxyl group), characterized by using an aqueous solvent containing at least water and a non-aqueous solvent capable of being separated from the aqueous solvent. Thus the reaction product is separated in the non-aqueous solvent layer and the imide compound catalyst or its changed product in the aqueous solvent layer, respectively.

公开(公告)号：JP2001286765A

公开(公告)日：2001-10-16

申请号：JP2000102795

申请日：2000-04-04

Applicant: DAICEL CHEM

Inventor： SHIMAMURA MASAMI ,  HIRAI NARIHISA ,  WATANABE HITOSHI

IPC: B01J31/40 ,  B01J31/02 ,  B01J38/00 ,  B01J38/52 ,  B01J38/60 ,  B01J38/64 ,  C07B61/00 ,  C07C27/12 ,  C07C29/50 ,  C07C35/08 ,  C07C45/33 ,  C07C49/403

Abstract: PROBLEM TO BE SOLVED: To provide a method for easily and efficiently regenerating a denatured imide based catalyst. SOLUTION: An imide based catalyst of N-hydroxyphthalimide on the like represented by formula (1) (in the formula, R1, R2 separately denote hydrogen atom, a halogen atom, or an alkyl and R1, R2 may be bonded to each other to form a double bond or an aromatic or non-aromatic cycle) and denatured by being used for reaction is hydrolyzed to be converted to a dicarboxylic acid represented by formula (2) (in the formula, R1, R2 are defined as described above) or its salt and then the obtained dicarboxylic acid or its salt or a reactive derivative of the dicarboxylic acid is reacted with (i) hydroxylamine or (ii) an o-substituted hydroxylamine and then treated with an acid to regenerate the imide based catalyst.

公开(公告)号：JP2001239171A

公开(公告)日：2001-09-04

申请号：JP2000055059

申请日：2000-02-29

Applicant: DAICEL CHEM

Inventor： HIRAI NARIHISA ,  WATANABE HITOSHI ,  SHIMAMURA MASAMI

IPC: B01J38/00 ,  B01J31/40 ,  C07B61/00 ,  C07C27/12 ,  C07C29/50 ,  C07C35/08 ,  C07C35/37 ,  C07C45/33 ,  C07C49/403 ,  C07C49/453

Abstract: PROBLEM TO BE SOLVED: To provide a method for efficiently separating an N-substituted cyclic imide-type catalyst or its decomposition products by using a simple means from a mixture of reaction products obtained in the presence of the N- substituted cyclic imide-type catalyst with either the N-substituted cyclic imide- type catalyst or its decomposition products. SOLUTION: The separation and recovery method of the present invention is to separate and recover an N-substituted cyclic imide-type catalyst or its decomposition products from a mixture of reaction products obtained in the presence of the N-substituted cyclic imide-type catalyst with either the N- substituted cyclic imide-type catalyst or its decomposition products. The N- substituted cyclic imide-type catalyst or its decomposition products are recovered as solids by precipitating or re-pulping the mixture in a solvent selected from a hydrocarbon, a chain type ether or water.