, where R=H, Br, Cl, F, CH3, includes a nucleophilic substitution of the chlorine atom in the 4-nitro-2-(trifluoromethyl)chlorobenzene when interacting with aniline or its corresponding derivative in solvent medium for 2.5 hours at 80°C and molar ratio of 2-nitro-4-(trifluoromethyl)chlorobenzene : 4-R-aniline = 2:1 and recovery of the resulting 2-nitro-N-[2-nitro-4-(trifluoromethyl)phenyl]-N-(4-(R)-phenyl)-4-(trifluoromethyl)aniline. Here, nucleophilic substitution is carried out by ultrasound in DMSO as the organic solvent, in the presence of tributylamine. Recovery of 2-itro-N-[2-nitro-4-(trifluoromethyl)phenyl]-N-(4-(R)-phenyl)-4-(trifluoromethyl)anilines is performed in a mixture of alcohol and 9% hydrochloric acid in volumetric ratio of 1:1, using electric current in a diaphragm cell in galvano-static mode in the presence of TiCl3, taken in the molar ratio of catalyst-carrier: dinitrosubstrate of 0.05:1, at a temperature of 40°C on lead cathode, while a passing a charge 12 F for 0.6 h through electrolytic cell, at current density of 9.45 A/dm2, 10% solution of sulfuric acid is used as the anolyte, platinum is used as the anode. The desired product is isolated.;EFFECT: method allows to obtain products with a high yield in a shorter time, carry out a nucleophilic substitution reaction in homogeneous conditions and is more economical sue to elimination of expensive agents and reduced amount of harmful waste.;10 ex"/> METHOD FOR PRODUCTION OF N<Sup>1</Sup>-2-AMINO-4-(TRIFLUOROMETHYL) PHENYL-N<Sup>1</Sup>-PHENYL-4-(TRIFLUOROMETHYL)-BENZENE-1,2-DIAMINE AND ITS DERIVATIVES
首页> 外国专利> METHOD FOR PRODUCTION OF N1-2-AMINO-4-(TRIFLUOROMETHYL) PHENYL-N1-PHENYL-4-(TRIFLUOROMETHYL)-BENZENE-1,2-DIAMINE AND ITS DERIVATIVES

METHOD FOR PRODUCTION OF N1-2-AMINO-4-(TRIFLUOROMETHYL) PHENYL-N1-PHENYL-4-(TRIFLUOROMETHYL)-BENZENE-1,2-DIAMINE AND ITS DERIVATIVES

机译:N 1 -[2-氨基-4-(三氟甲基)苯基]的制备方法-N 1 -苯基-4-(三氟甲基)-苯-1,2胺及其衍生物

摘要

FIELD: pharmacology.;SUBSTANCE: invention relates to a method for preparation of N1-[2-amino-4-(trifluoromethyl) phenyl]-N1phenyl-4-(trifluoromethyl)benzene-1,2-diamine and its derivatives of the general formula (I). The derived compounds can be used for synthesis of aromatic polyimides, finding application in various advanced technologies for semiconductor packages, electronic circuits, fuel cells, liquid crystal displays (LCD), for gas separation using polymeric membranes. Methods for preparation of N1-[2-amino-4-(trifluoromethyl)phenyl]-N1-phenyl-4-(trifluoromethyl)benzene-1,2-diamine and its derivatives of the general formula , where R=H, Br, Cl, F, CH3, includes a nucleophilic substitution of the chlorine atom in the 4-nitro-2-(trifluoromethyl)chlorobenzene when interacting with aniline or its corresponding derivative in solvent medium for 2.5 hours at 80°C and molar ratio of 2-nitro-4-(trifluoromethyl)chlorobenzene : 4-R-aniline = 2:1 and recovery of the resulting 2-nitro-N-[2-nitro-4-(trifluoromethyl)phenyl]-N-(4-(R)-phenyl)-4-(trifluoromethyl)aniline. Here, nucleophilic substitution is carried out by ultrasound in DMSO as the organic solvent, in the presence of tributylamine. Recovery of 2-itro-N-[2-nitro-4-(trifluoromethyl)phenyl]-N-(4-(R)-phenyl)-4-(trifluoromethyl)anilines is performed in a mixture of alcohol and 9% hydrochloric acid in volumetric ratio of 1:1, using electric current in a diaphragm cell in galvano-static mode in the presence of TiCl3, taken in the molar ratio of catalyst-carrier: dinitrosubstrate of 0.05:1, at a temperature of 40°C on lead cathode, while a passing a charge 12 F for 0.6 h through electrolytic cell, at current density of 9.45 A/dm2, 10% solution of sulfuric acid is used as the anolyte, platinum is used as the anode. The desired product is isolated.;EFFECT: method allows to obtain products with a high yield in a shorter time, carry out a nucleophilic substitution reaction in homogeneous conditions and is more economical sue to elimination of expensive agents and reduced amount of harmful waste.;10 ex
机译:N 1 -[2-氨基-4-(三氟甲基)苯基] -N 1 苯基-4的制备方法-(三氟甲基)苯-1,2-二胺及其通式(I)的衍生物。衍生的化合物可用于合成芳族聚酰亚胺,并在各种先进技术中得到应用,这些技术用于半导体封装,电子电路,燃料电池,液晶显示器(LCD),以及使用聚合物膜进行气体分离。 N 1 -[2-氨基-4-(三氟甲基)苯基] -N 1 -苯基-4-(三氟甲基)苯-1,2-的制备方法二胺及其通式的衍生物,其中R = H,Br,Cl,F CH 3 在80°C时与苯胺或其相应衍生物在溶剂介质中相互作用2.5小时,并包括4-硝基-2-(三氟甲基)氯苯中氯原子的亲核取代。 2-硝基-4-(三氟甲基)氯苯的摩尔比∶4-R-苯胺= 2∶1,回收得到的2-硝基-N- [2-硝基-4-(三氟甲基)苯基] -N-( 4-(R)-苯基)-4-(三氟甲基)苯胺。在此,在三丁胺的存在下,在有机溶剂DMSO中通过超声波进行亲核取代。在乙醇和9%盐酸的混合物中回收2-硝基-N- [2-硝基-4-(三氟甲基)苯基] -N-(4-(R)-苯基)-4-(三氟甲基)苯胺在TiCl 3 存在的情况下,在电流模式下,在隔膜电池中通过电流以静态比率,使酸的比例为1:1,催化剂-载体:二硝基底物的摩尔比为0.05:1 ,在铅阴极上温度为40°C的同时,使12 F的电荷通过电解池0.6 h,在电流密度为9.45 A / dm 2 的情况下,硫酸的浓度为10%用作阳极液,铂用作阳极。效果:该方法允许在较短的时间内获得高收率的产品,在均相条件下进行亲核取代反应,并且在消除昂贵试剂和减少有害废物量方面更经济。 10前

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