第 35 卷第 4 期 |  | Vol. 35 No. 4 | 2005 年 8 月 | Aug 2005 |
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所屬欄目:農藥及中間體
肼解還原法合成2,6-二氯-4-三氟甲基苯胺 |
蘭艷娜; 張華; 徐強; 李亞明; 羅麗梅; 叢麗英(大連理工大學(xué)精細化工國家重點(diǎn)實(shí)驗室; 遼寧大連) |
摘 要:以3,4,5-三氯三氟甲苯為起始原料,經(jīng)肼解、還原合成目的產(chǎn)物2,6-二氯-4-三氟甲基苯胺,總收率為81%?疾炝巳軇、物料配比、反應溫度和反應時(shí)間對肼解反應的影響,對目的產(chǎn)物采用紅外光譜、1H核磁共振波譜、氣相色譜/質(zhì)譜進(jìn)行結構鑒定,證明結構正確。 |
關(guān)鍵詞:2; 6-二氯-4-三氟甲基苯胺; 3; 4; 5-三氯三氟甲苯; 肼解; 結構表征 |
中圖分類(lèi)號:TQ246.3 文獻標識碼:A 文章編號: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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