公开(公告)号：JPS59134753A

公开(公告)日：1984-08-02

申请号：JP525183

申请日：1983-01-18

Applicant: Mitsui Toatsu Chem Inc

Inventor： YAMAGUCHI KEISABUROU ,  SUGIMOTO KENICHI ,  TANABE YOSHIMITSU ,  KAWASHIMA SABUROU ,  YAMAGUCHI TERUHIRO

IPC: C07B61/00 ,  B01J23/00 ,  B01J23/40 ,  B01J23/70 ,  B01J25/00 ,  C07C67/00 ,  C07C209/00 ,  C07C211/21 ,  C07C211/50

CPC classification number: Y02P20/52

Abstract: PURPOSE: To obtain the titled compound useful as a monomer for high polymer, etc. safely and economically, by subjecting 3,3'-diaminobenzophenone or 3,4'- diaminobenzophenone to catalytic reduction in an aqueous solution of mineral acid under relatively mild conditions.
CONSTITUTION: 3,3-Diaminobenzophenone or 3,4'-diaminobenzophenone is subjected to catalytic reduction in an aqueous solution of mineral acid (preferably sulfuric acid, or hydrochloric acid) preferably in the presence of a palladium or platinum catalyst industrially at 20W150°C at normal pressure W100kg/cm
2 to give the desired compound. An amount of the mineral acid used is 0.1W4 equivalent, preferably 1W2.5 equivalent based on diaminobenzophenone of raw material. The concentration of the aqueous solution of the mineral acid is 0.05W12 normality, preferably 0.5W4 normality. An amount of the catalyst used is properly 0.01W20wt% calculated as metal based on the raw material.
COPYRIGHT: (C)1984,JPO&Japio

Abstract translation: 目的：通过在相对温和的条件下，使3,3'-二氨基二苯甲酮或3,4'-二氨基二苯甲酮在无机酸水溶液中进行催化还原，得到安全，经济地用作高分子单体的标题化合物 。 构成：3,3-二氨基二苯甲酮或3,4'-二氨基二苯甲酮在无机酸（优选硫酸或盐酸）的水溶液中优选在工业上在20-150℃的钯或铂催化剂存在下进行催化还原 在常压-100kg / cm 2下，得到所需化合物。 无机酸的使用量相对于原料的二氨基二苯甲酮为0.1-4当量，优选为1-2.5当量。 无机酸水溶液的浓度为0.05-12正常值，优选为0.5-4正常值。 所使用的催化剂的量相当于以原料为基准计算为0.01-20wt％的金属。

公开(公告)号：JPS58203946A

公开(公告)日：1983-11-28

申请号：JP8489082

申请日：1982-05-21

Applicant: Mitsui Toatsu Chem Inc

Inventor： TANABE YOSHIMITSU ,  YAMAGUCHI KEISABUROU ,  SUGIMOTO KENICHI ,  KAWASHIMA SABUROU ,  YAMAGUCHI TERUHIRO

IPC: C07C201/08 ,  C07C67/00 ,  C07C201/00 ,  C07C205/45 ,  C07C313/00 ,  C07C315/04 ,  C07C317/14

Abstract: PURPOSE: To obtain the titled compound useful as an intermediate for agricultural chemicals, medicines and raw material for heat-resistant resins, etc., by nitrating 4,4'-dichlorobenzophenone, etc. in an aliphatic halogenated hydrocarbon as a solvent.
CONSTITUTION: 4,4'-Dichlorobenzophenone or 4,4'-dichlorodiphenyl sulfone is nitrated with a mixed acid or a nitrate and sulfuric acid in an aliphatic halogenated hydrocarbon solvent in an amount of 1W10 times or the weight of the raw material at 20W100°C, preferably 40W80°C, to give the aimed crystalline compound. Preferably, the nitric acid having 1.45W1.50 specific gravity in a molar amount of 2.2W3.0 times of that of the raw material or the nitrate in a molar amount of 2.1W2.5 times of that of the raw material is used.
EFFECT: The heat of reaction is easily controlled, and the amount of the mixed acid can be reduced. The reaction mixture is easily post-treated.
COPYRIGHT: (C)1983,JPO&Japio

Abstract translation: 目的：通过在脂肪族卤代烃作为溶剂中硝化4,4'-二氯二苯甲酮等，获得用作农药，药物和耐热树脂的原料的中间体的标题化合物。 构成：将4,4'-二氯二苯甲酮或4,4'-二氯二苯基砜与脂肪族卤代烃溶剂中的混合酸或硝酸盐和硫酸硝化，其量为1-10倍或原料重量 20-100℃，优选40-80℃，得到目标结晶化合物。 优选使用摩尔量为原料的2.2〜3.0倍的比重为1.45〜1.50的硝酸，或者摩尔量为原料的2.1〜2.5倍的硝酸盐的硝酸。 效果：容易控制反应热，可以减少混合酸的量。 反应混合物容易后处理。

公开(公告)号：JPS59172441A

公开(公告)日：1984-09-29

申请号：JP4709783

申请日：1983-03-23

Applicant: Mitsui Toatsu Chem Inc

Inventor： YAMAGUCHI KEISABUROU ,  SUGIMOTO KENICHI ,  TANABE YOSHIMITSU ,  KAWASHIMA SABUROU ,  YAMAGUCHI TERUHIRO

IPC: C07B61/00 ,  B01J23/00 ,  B01J23/40 ,  B01J23/70 ,  B01J25/02 ,  B01J27/00 ,  B01J27/02 ,  B01J27/08 ,  C07C20060101 ,  C07C67/00 ,  C07C201/00 ,  C07C205/45 ,  C07C221/00 ,  C07C225/22

CPC classification number: C07C201/14 ,  C07C221/00 ,  C07C205/45 ,  C07C225/22

Abstract: PURPOSE: To obtain the titled compound industrially advantageously, by using 3- or 4-nitrobenzoyl chloride and chlorobenzene as starting substances, subjecting them to three-stage processes of Friedel-Crafts reaction, nitration reaction and reduction, and dehydrochlorination.
CONSTITUTION: 3- or 4-Nitrobenzoyl chloride and chlorobenzene are subjected to Friedel-Crafts reaction in the presence of a Lewis acid catalyst to give a mixture of isomers of chloronitrobenzophenone. This compound without purification is nitrated to give a mixture of chloro-dinitrobenzophenone. This compound is reduced catalytically and dechlorinated in the presence of a reductive catalyst and a dehydrochlorinating agent, to give 3,3'- or 3,4'-diaminobenzophenone useful as a monomer for heat-resistant high polymers, intermediate for agricultural chemicals, drugs, etc. in high yield in high purity and industrially inexpensively.
COPYRIGHT: (C)1984,JPO&Japio

Abstract translation: 目的：通过使用3-或4-硝基苯甲酰氯和氯苯作为起始物质，在工业上有利地得到标题化合物，进行Friedel-Crafts反应，硝化反应和还原的三步法和脱氯化氢。 构成：在路易斯酸催化剂存在下，将3-或4-硝基苯甲酰氯和氯苯进行Friedel-Crafts反应，得到氯二硝基苯甲酮异构体的混合物。 将不经纯化的该化合物硝化，得到氯二硝基二苯甲酮的混合物。 该化合物在还原催化剂和脱氯化氢剂的存在下催化还原脱氯，得到3,3'-或3,4'-二氨基二苯甲酮，其可用作耐高温聚合物的单体，农药中间体，药物 等，高纯度，工业上廉价。

公开(公告)号：JPS59116260A

公开(公告)日：1984-07-05

申请号：JP22497782

申请日：1982-12-23

Applicant: Mitsui Toatsu Chem Inc

Inventor： YAMAGUCHI KEISABUROU ,  SUGIMOTO KENICHI ,  TANABE YOSHIMITSU ,  KAWASHIMA SABUROU ,  YAMAGUCHI TERUHIRO

IPC: C07B61/00 ,  B01J23/00 ,  B01J23/42 ,  B01J23/44 ,  B01J23/755 ,  B01J27/00 ,  B01J27/08 ,  B01J31/00 ,  B01J31/02 ,  C07C67/00 ,  C07C313/00 ,  C07C315/04 ,  C07C317/36

CPC classification number: Y02P20/52

Abstract: PURPOSE:To obtain the titled compound useful as agricultural chemicals, etc. industrially advantageously, by nitrating a reaction mixture of 4-chlorobenzenesulfonic acid, etc. and chlorobenzene to give an isomer mixture, reducing it catalytically without separating and purifying it, followed by dehydrochlorinating the reaction product. CONSTITUTION:A reaction mixture obtained by reacting 4-chloro-benzenesulfonic acid or 4-chlorobenzenesulfonyl chloride and benzene is nitrated using mixed acid, fuming nitric acid, etc. as a nitrating agent, to give a mixture of dinitrodichlorodiphenylsulfone. It is then reduced catalytically, and dehydrochlorinated in the presence of a reducing catalyst (e.g., Ni, Pd, etc.) and a dehydrochlorinating agent (e.g., CaCO3, NaOH, MgO, etc.), to give 3, 3'-diaminodiphenyl- sulfone. An isomer mixture obtained by the nitration does not need separation and purification and the desired substance is obtained in high yield.

Abstract translation: 目的：通过硝化4-氯苯磺酸等与氯苯的反应混合物得到异构体混合物，得到可用于农药的标题化合物，有利于工业化，得到异构体混合物，催化还原，不分离和纯化，然后脱氯化氢 反应产物。 构成：使用混合酸，发烟硝酸等作为硝化剂将4-氯 - 苯磺酸或4-氯苯磺酰氯与苯反应得到的反应混合物硝化，得到二硝基二氯二苯砜的混合物。 然后在还原催化剂（例如Ni，Pd等）和脱氯化氢剂（例如CaCO 3，NaOH，MgO等）存在下催化还原并脱氯化氢，得到3,3-二氨基二苯 - 砜。 通过硝化获得的异构体混合物不需要分离和纯化，并且以高产率获得所需物质。

公开(公告)号：JPS5955855A

公开(公告)日：1984-03-31

申请号：JP16665682

申请日：1982-09-27

Applicant: Mitsui Toatsu Chem Inc

Inventor： YAMAGUCHI KEISABUROU ,  SUGIMOTO KENICHI ,  TANABE YOSHIMITSU ,  KAWASHIMA SABUROU ,  YAMAGUCHI TERUHIRO

IPC: C07B61/00 ,  B01J23/00 ,  C07C67/00 ,  C07C209/00 ,  C07C209/10 ,  C07C209/36 ,  C07C211/50 ,  C07C211/54

CPC classification number: C07C209/36

Abstract: PURPOSE: To obtain 3,3'-diaminodiphenylmethane useful as an intermediate for agricultural chemicals, drugs, etc., in high yield industrially advantageously, by reducing catalytically and dechlorinating a specific dinitrobenzophenone in the presence of a reducing catalyst.
CONSTITUTION: A benzophenone compound shown by the formula I (X
1 and X
2 are H, or Cl; with the proviso that a case where both are Cl is omitted) is nitrated, to give a dinitrobenzophenone shown by the formula II. The prepared dinitorbenzophenone shown by the formula II is reduced catalytically and dechlorinated in the presence of a reducing catalyst(e.g., Ni, Pt, Co, etc.) in an organic solvent such as methanol, etc., to give 3,3'-diaminophenylmethane. The reaction is carried out preferably at 20W200°C reaction temperature at normal pressure W50kg/cm
2 .
EFFECT: Neigher problem of environmental pollution resulting from waste is caused, nor complicated purifying process is required.
COPYRIGHT: (C)1984,JPO&Japio

Abstract translation: 目的：在还原催化剂存在下，通过在特定的二硝基二苯甲酮中进行催化脱氯和脱氯，得到3,3'-二氨基二苯基甲烷作为农药，药物等中间产物的高产率。 构成：将式I所示的二苯甲酮化合物（X1和X2为H或Cl，条件是省略了两者均为Cl的情况）硝化，得到式II所示的二硝基二苯甲酮。 在有机溶剂如甲醇等中，在还原催化剂（例如Ni，Pt，Co等）存在下，将式II所示的制备的二硝基二苯甲酮催化还原脱氯，得到3,3'- 二氨基苯基甲烷。 反应优选在20-200℃的反应温度在常压-50kg / cm 2下进行。 影响：造成污染环境污染的问题较严重，不需要复杂的净化过程。

公开(公告)号：JPS5916860A

公开(公告)日：1984-01-28

申请号：JP12377582

申请日：1982-07-17

Applicant: Mitsui Toatsu Chem Inc

Inventor： YAMAGUCHI KEISABUROU ,  SUGIMOTO KENICHI ,  TANABE YOSHIMITSU ,  KAWASHIMA SABUROU ,  YAMAGUCHI TERUHIRO

IPC: C07B61/00 ,  B01J23/00 ,  B01J23/40 ,  B01J23/70 ,  B01J25/00 ,  C07C67/00 ,  C07C213/00 ,  C07C221/00 ,  C07C225/22

CPC classification number: Y02P20/52

Abstract: PURPOSE: To obtain the titled compound industrially advantageously, by nitrating a reaction mixture of 2-chlorobenzoyl chloride, etc. and chlorobenzene, reducing catalytically it in the presence of a reducing catalyst and a dehydrochlorinating agent, dechlorinating it.
CONSTITUTION: A reaction mixture obtained by Friedel-Crafts reaction of 2- chlorobenzoyl chloride and/or 4-chlorobenzoyl chloride and chlorobenzene is nitrated to give a mixture of dinitrodichloro-benzophenone, which is subjected to catalytic reduction in the presence of a reducing catalyst (e.g., Ni, or Pd) and a dehydrochlorinating agent (e.g., NaOH), and dechlorinated, to give 3,3'-diaminobenzophenone. The nitration is carried out using a common nitrating agent (e.g., mixed acid, fuming nitric acid) at 50W100°C for 2W10hr, the intermediate is not isolated, and the reduction of nitro group and the dechlorination are carried out successively or simultaneously.
COPYRIGHT: (C)1984,JPO&Japio

Abstract translation: 目的：为了得到工业上有用的标题化合物，通过硝化2-氯苯甲酰氯等与氯苯的反应混合物，在还原催化剂和脱氯化氢剂的存在下催化还原，对其进行脱氯。 构成：将通过2-氯苯甲酰氯和/或4-氯苯甲酰氯和氯苯的Friedel-Crafts反应获得的反应混合物进行硝化，得到二硝基二氯 - 二苯甲酮的混合物，其在还原催化剂存在下进行催化还原 例如Ni或Pd）和脱氯化氢剂（例如NaOH）并脱氯，得到3,3'-二氨基二苯甲酮。 使用普通硝化剂（例如，混合酸，发烟硝酸）在50-100℃进行2-10小时的硝化，中间体不分离，硝基还原和脱氯进行 连续地或同时地

公开(公告)号：JPS58177946A

公开(公告)日：1983-10-18

申请号：JP6027382

申请日：1982-04-13

Applicant: Mitsui Toatsu Chem Inc

Inventor： YAMAGUCHI KEISABUROU ,  SUGIMOTO KENICHI ,  TANABE YOSHIMITSU ,  KAWASHIMA SABUROU ,  YAMAGUCHI TERUHIRO

IPC: C07C225/22 ,  B01J23/40 ,  B01J25/02 ,  C07B61/00 ,  C07C221/00

CPC classification number: Y02P20/52

Abstract: PURPOSE: To prepare the titled compound useful as a monomer of a heat-resistant polymer, etc., economically, in high yield, by the catalytic reduction and dehalogenation of a benzophenone compound in the presence of a reduction catalyst and a dehydrohalogenating agent.
CONSTITUTION: A benzophenone compound of formula (X and Y are halogen atom) is subjected to the catalytic reduction and dehalogenation in the presence of a reduction catalyst (e.g. Ni, Pd, etc.) and a dehydrohalogenating agent (e.g. CaCO
3 , NaOH, etc.) to obtain the objective 3,3'-diaminobenzophenone. The reaction is carried out usually in a reaction solvent (e.g. methanol) at 20W 200°C, especially 20W100°C under atmospheric pressure W about 50kg/cm
2 .G. There is no environmental pollution with wastes, and a high-purity product can be obtained without using purification process.
COPYRIGHT: (C)1983,JPO&Japio

Abstract translation: 目的：为了通过在还原催化剂和脱卤化氢剂的存在下，通过二苯甲酮化合物的催化还原和脱卤，以高产率经济地制备可用作耐热聚合物单体的标题化合物。 构成：在还原催化剂（例如Ni，Pd等）和脱卤化氢剂（例如CaCO 3，NaOH等）的存在下，将式（X和Y为卤素原子）的二苯甲酮化合物进行催化还原和脱卤 。）得到目标3,3'-二氨基二苯甲酮。 反应通常在反应溶剂（如甲醇）中，在20-200℃，特别是20-100℃，常压下，约50kg / cm 2 .G。 废弃物无环境污染，无需纯化工艺即可获得高纯度产品。

公开(公告)号：JPS58181686A

公开(公告)日：1983-10-24

申请号：JP6469582

申请日：1982-04-20

Applicant: Mitsui Toatsu Chem Inc

Inventor： YAMAGUCHI TERUHIRO ,  KAWASHIMA SABUROU ,  YAMAGUCHI KEISABUROU ,  SUGIMOTO KENICHI ,  TANABE YOSHIMITSU

IPC: B41M5/333

CPC classification number: B41M5/3335

Abstract: PURPOSE:To obtain a recording sheet with a gradation property which is better in the rising of the color development density at the moment of heating by using one or more kinds of specified 2, 2'-methylene diphenyl compounds as developer for a thermal recording sheet. CONSTITUTION:2,2'-methylenediphenol compound as given by the formula (where, R represents hydrogen, alkyl group with C1-C12, cycloalkyl group with C3- C10, alalkyl group or phenyl group with C7-C10, which may be identical or different) and a coloring agent developing color by a melt reaction with the developer are separately dissolved or dispersed in water or a solvent and mixed together. An appropriate binder is added to the mixture and the mixed liquid thus obtained is applied on a supporting body such as paper and synthetic resin film and dried. The quantities of the components shall be 1-15pt.wt. for the coloring agent, 1-95pt.wt. for the developer of the formula and 1-40pt.wt. for the binder.

Abstract translation: 目的：通过使用一种或多种指定的2,2'-亚甲基二苯基化合物作为热敏记录片材的显影剂，获得在加热时色调发展密度上升时更好的渐变性的记录片材 。 构成：由式（其中，R表示氢，具有C 1 -C 12的烷基，具有C 3 -C 10的环烷基，具有C 7 -C 10的烷基或具有C 7 -C 10的苯基）的2,2'-亚甲基二苯酚化合物，其可以相同或 不同的）和通过与显影剂的熔融反应显色的着色剂分别溶解或分散在水或溶剂中并混合在一起。 将合适的粘合剂加入到混合物中，并将如此获得的混合液施加到诸如纸和合成树脂膜的支撑体上并干燥。 组件的数量应为1-15pt.wt。 对于着色剂，1-95pt.wt。 对于公式的开发者和1-40pt.wt。 用于粘合剂。