第 36 卷第 4 期 |  | Vol. 36 No. 4 | 2006 年 8 月 | Aug 2006 |
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所屬欄目:醫藥及中間體
3-甲硫基苯胺的制備 |
任戎; 張翌; 劉登科; 王松青(天津大學(xué)藥物科學(xué)與技術(shù)學(xué)院; 天津藥物研究院; 天津300072天津藥物研究院) |
摘 要:以硝基苯為起始原料,經(jīng)氯磺化反應、還原反應(KI/H3PO3)、還原反應(Na2S)、甲基化反應、還原反應(Fe/HCl),制得3-甲硫基苯胺(1)。優(yōu)化了反應條件,簡(jiǎn)化了操作,總收率50.3%,純度99.1%(HPLC)。 |
關(guān)鍵詞:3-甲硫基苯胺; 還原反應; 制備; 雙(3-硝基苯基)二硫化物 |
中圖分類(lèi)號:TQ246.3+2 文獻標識碼:A 文章編號:1009-9212(2006)04-0016-02 |
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Preparation of 3-(Methylthio)benzenamine |
REN Rong1; 2; ZHANG Yi1; LIU Deng-ke2; WANG Song-qing1 (1. College of Pharmaceuticals and Biotechnology; Tianjin University; Tianjin 300072; China; 2. Tianjin Institute of Pharmaceutical Research; Tianjin 300193; China) |
Abstract:3-(Methylthio)benzenamine(1)was obtained from nitrobenzene through 5-step reactions including chlorosulfonation,reduction with KI/H3PO3,reduction with Na2S,methylation and reduction with Fe/HCl. The overall yield was 50.3%,and purity 99.1%(HPLC). The procedure developed had several advantages of facile reaction conditions,convenient operation and cheap reagents. |
Key words:3-(methylthio)benzenamine; reduction; preparation; bis(3-nitrophenyl)disulfide |
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基金項目:天津市科委基礎科學(xué)重點(diǎn)資助項目(033801911)
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收稿日期:2006-05-09
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