对以邻硝基甲苯为主要原料,经锌粉 氯化铵溶液还原、氯甲酸甲酯酰基化、硫酸二甲酯甲基化合成N 甲氧基 N 2 甲基苯基氨基甲酸甲酯的工艺路线进行了研究.重点考察了还原反应中溶剂种类、还原温度对反应的影响以及N 羟基 N 2 甲苯氨基甲...对以邻硝基甲苯为主要原料,经锌粉 氯化铵溶液还原、氯甲酸甲酯酰基化、硫酸二甲酯甲基化合成N 甲氧基 N 2 甲基苯基氨基甲酸甲酯的工艺路线进行了研究.重点考察了还原反应中溶剂种类、还原温度对反应的影响以及N 羟基 N 2 甲苯氨基甲酸甲酯的纯化方法.N 羟基 N 2 甲苯基氨基甲酸甲酯、N 甲氧基 N 2 甲苯基氨基甲酸甲酯均经MS,1HNMR确认.展开更多
Bis(2-benzimidazolyl)propane was synthesized by the reaction of o-phenylenediamine and glutaric acid which was accelerated by microwave irradiation and catalyzed by poly phosphoric acid(PPA) under solvent-free conditi...Bis(2-benzimidazolyl)propane was synthesized by the reaction of o-phenylenediamine and glutaric acid which was accelerated by microwave irradiation and catalyzed by poly phosphoric acid(PPA) under solvent-free condition. By the method of orthogonal experiment optimize synthesis factors which affect the reation: o-Phenylent Diamine: glutaric acid:2.2∶1.0(mol:mol),PPA:9.0g,time of microwave irradiation:8min, and the power of microwave irradiation:160W. Under the optimal condition, the highest yield of Bis(2-benzimidazolyl) propane is 77.4%. The products were characterized by melting point determination, IR spectrogram,1HNMR spectra and 13CNMR spectra.展开更多
文摘对以邻硝基甲苯为主要原料,经锌粉 氯化铵溶液还原、氯甲酸甲酯酰基化、硫酸二甲酯甲基化合成N 甲氧基 N 2 甲基苯基氨基甲酸甲酯的工艺路线进行了研究.重点考察了还原反应中溶剂种类、还原温度对反应的影响以及N 羟基 N 2 甲苯氨基甲酸甲酯的纯化方法.N 羟基 N 2 甲苯基氨基甲酸甲酯、N 甲氧基 N 2 甲苯基氨基甲酸甲酯均经MS,1HNMR确认.
文摘Bis(2-benzimidazolyl)propane was synthesized by the reaction of o-phenylenediamine and glutaric acid which was accelerated by microwave irradiation and catalyzed by poly phosphoric acid(PPA) under solvent-free condition. By the method of orthogonal experiment optimize synthesis factors which affect the reation: o-Phenylent Diamine: glutaric acid:2.2∶1.0(mol:mol),PPA:9.0g,time of microwave irradiation:8min, and the power of microwave irradiation:160W. Under the optimal condition, the highest yield of Bis(2-benzimidazolyl) propane is 77.4%. The products were characterized by melting point determination, IR spectrogram,1HNMR spectra and 13CNMR spectra.
