| 第 36 卷第 2 期 |  | Vol. 36 No. 2 | | 2006 年 4 月 | Apr 2006 |
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所屬欄目：醫藥及中間體
2-甲基氨基硫脲的合成 |
| 薛堯森; 畢彩豐; 馬少華; 華哲(中國海洋大學(xué)化學(xué)化工學(xué)院; 山東青島) |
| 摘 要：以水合肼和亞磷酸二甲酯為起始原料合成甲基肼,再直接和硫氰酸銨反應兩步制取2-甲基氨基硫脲。詳細研究并得到兩步反應的優(yōu)化條件:甲基化反應以四丁基溴化銨為催化劑,反應溫度為110-120℃,反應時(shí)間為2h;后一步反應原料配比n(甲基肼)∶n(硫氰酸銨)=1∶1.2,熱重排溫度為120℃左右,熱重排時(shí)間為2h。在此條件下總收率達45.5%(以水合肼計)。 |
| 關(guān)鍵詞：2-甲基氨基硫脲; 甲基肼; 合成 |
| 中圖分類(lèi)號：TQ225.27 文獻標識碼：A 文章編號：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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