肼解还原法合成2,6-二氯-4-三氟甲基苯胺

Synthesis of 2,6-Dichloro-4-Trifluoromethylaniline with Hydrazinolysis and Hydrogenolysis Reduction

以3,4,5-三氯三氟甲苯为起始原料,经肼解、还原合成目的产物2,6-二氯-4-三氟甲基苯胺,总收率为81%。考察了溶剂、物料配比、反应温度和反应时间对肼解反应的影响,对目的产物采用红外光谱、1H核磁共振波谱、气相色谱/质谱进行结构鉴定,证明结构正确。

2,6-dichloro-4-trifluoromethylphenylhydrazine was prepared by hydrazinolysis of 3,4,5-trichloro - benzotrifluoride with hydrazine hydrate, reduced by hydrogen gas with Raney Ni as catalyst to give 2,6-dichloro- 4-trifluoromethylaniline.Under the optimum condition the total yield of 2,6-dichloro-4-trifluoromethylphenylhy drazine was up to 81%. The effects of temperature, material mixture ratio and reaction time on the hydrazinolysis were also discussed. The structure of the compound was confirmed by spectral characterizations.