第 35 卷第 4 期 | | Vol. 35 No. 4 | 2005 年 8 月 | Aug 2005 |
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所属栏目:农药及中间体
肼解还原法合成2,6-二氯-4-三氟甲基苯胺 |
兰艳娜; 张华; 徐强; 李亚明; 罗丽梅; 丛丽英(大连理工大学精细化工国家重点实验室; 辽宁大连) |
摘 要: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。 |
关键词:2; 6-二氯-4-三氟甲基苯胺; 3; 4; 5-三氯三氟甲苯; 肼解; 结构表征 |
中图分类号:TQ246.3 文献标识码:A 文章编号:1009-9212(2005)04-0030-03 |
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Synthesis of 2,6-Dichloro-4-Trifluoromethylaniline with Hydrazinolysis and Hydrogenolysis Reduction |
LAN Yan-na; ZHANG Hua; XU Qiang; LI Ya-ming; LUO Li-mei; CONG Li-ying (State Key Laboratory of Fine Chemicals; Dalian Uiniversity of Technology; Dalian 116012; China ) |
Abstract: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 c... |
Key words:2; 6-dichloro-4-trifluoromethylaniline; 3; 4; 5-trichloro-benzotrifluoride; hydrazinolysis; characterization |
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收稿日期:2005-04-20
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