| 2-甲基氨基硫脲的合成 |
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| 引用本文： | 薛尧森,毕彩丰,马少华,华哲. 2-甲基氨基硫脲的合成[J]. 精细化工中间体, 2006, 36(2): 34-35 |
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| 作者姓名： | 薛尧森 毕彩丰 马少华 华哲 |
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| 作者单位： | 中国海洋大学,化学化工学院,山东,青岛,266003 |
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| 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)。
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| 关 键 词： | 2-甲基氨基硫脲 甲基肼 合成 |
| 文章编号： | 1009-9212(2006)02-0034-02 |
| 收稿时间： | 2005-11-02 |
| 修稿时间： | 2005-11-02 |
Synthesis of 2-Methylthiosemicarbazide |
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| XUE Yao-sen,BI Cai-feng,MA Shao-hua,HUA Zhe. Synthesis of 2-Methylthiosemicarbazide[J]. Fine Chemical Intermediates, 2006, 36(2): 34-35 |
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| Authors: | XUE Yao-sen BI Cai-feng MA Shao-hua HUA Zhe |
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| Affiliation: | College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266003, China |
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| 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 temperature 120 ℃,and the time 2 h. The total yield of 2-methyl-thiosemicarbazide was 45.5% based on hydrazine. |
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| Keywords: | 2-methylthiosemicarbazide methyl hydrazine synthesis |
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