| 第 36 卷第 2 期 |  | Vol. 36 No. 2 | | 2006 年 4 月 | Apr 2006 |
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所属栏目：医药及中间体
2-甲基氨基硫脲的合成 |
| 薛尧森; 毕彩丰; 马少华; 华哲(中国海洋大学化学化工学院; 山东青岛) |
| 摘 要：以水合肼和亚磷酸二甲酯为起始原料合成甲基肼,再直接和硫氰酸铵反应两步制取2-甲基氨基硫脲。详细研究并得到两步反应的优化条件:甲基化反应以四丁基溴化铵为催化剂,反应温度为110-120℃,反应时间为2h;后一步反应原料配比n(甲基肼)∶n(硫氰酸铵)=1∶1.2,热重排温度为120℃左右,热重排时间为2h。在此条件下总收率达45.5%(以水合肼计)。 |
| 关键词：2-甲基氨基硫脲; 甲基肼; 合成 |
| 中图分类号：TQ225.27 文献标识码：A 文章编号：1009-9212(2006)02-0034-02 |
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| Synthesis of 2-Methylthiosemicarbazide |
| XUE Yao-sen; BI Cai-feng; MA Shao-hua; HUA Zhe（College of Chemistry and Chemical Engineering; Ocean University of China; Qingdao 266003; China） |
| Abstract：2-methylthiosemicarbazide was synthesized via two steps. Methyl hydrazine was synthesized from hydrazine and dimethyl phosphite,and then directly reacted with ammonium thiocyanate to obtain the target material. The optimal conditions were obtained as follows: methylated reaction was carried out in the presence of n-Bu4NBr as catalyst,the reaction temperature 110~120 ℃,and reaction time 2 h. The molar ratio of methyl hydrazine to ammonium thiocyanate was 1 ∶ 1.2 in the next step,the heat rearrangement temper... |
| Key words：2-methylthiosemicarbazide; methyl hydrazine; synthesis |
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收稿日期：2005-11-02
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