| 1,1-二甲硫基-2-硝基乙烯的合成 |
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| 引用本文： | 贾正桂.1,1-二甲硫基-2-硝基乙烯的合成[J].精细化工中间体,2006,36(1):52-54. |
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| 作者姓名： | 贾正桂 |
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| 作者单位： | 淮阴师范学院,化学系,江苏,淮安,223001 |
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| 摘 要： | 研究了以硝基甲烷和二硫化碳为原料,合成1,1-二甲硫基-2-硝基乙烯。考察了反应温度、反应时间、甲基化试剂、溶剂、投料比等对于反应产物的影响,得到优化工艺条件为:反应温度35℃,反应时间3h。以硫酸二甲酯为甲基化试剂,常温下反应时间3 h,重结晶得1,1-二甲硫基-2-硝基乙烯,收率为84%,产物通过IR、1H-NMR鉴定。
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| 关 键 词： | 1 1-二甲硫基-2-硝基乙烯 中间体 合成 |
| 文章编号： | 1009-9212(2006)01-0052-03 |
| 收稿时间： | 2005-09-26 |
| 修稿时间： | 2005年9月26日 |
Synthesis of 1,1-bis(methylthio)-2-nitroethene |
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| JIA Zheng-gui.Synthesis of 1,1-bis(methylthio)-2-nitroethene[J].Fine Chemical Intermediates,2006,36(1):52-54. |
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| Authors: | JIA Zheng-gui |
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| Abstract: | 1,1-bis(methylthio)-2-nitroethene was prepared by reacting nitromethane and carbon bisulfide.Effects of temperature,reaction time,methylating agent,solvent,molar ratio of nitromethane and carbon bisulfide on yield of 1,1-bis(methylthio)-2-nitroethane were discussed.The optimum operation conditions were as follow: the reaction temperature of 35 ℃,reaction time for 3.0 h.In the process of dimethyl sulfate methylation,the optimum operation condition was at the room temperature for 3.0 h.The yield was 84%.Crude product was purified by re-crystallization.1,1-Bis(methylthio)-2-nitroethene was identified by IR and 1H-NMR. |
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| Keywords: | 1 1-bis(methylthio)-2-nitroethene intermediate product synthesis |
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