第 36 卷第 1 期 | | Vol. 36 No. 1 | 2006 年 2 月 | Feb 2006 |
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所属栏目:有机合成原料
1,1-二甲硫基-2-硝基乙烯的合成 |
贾正桂(淮阴师范学院化学系; 江苏淮安) |
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。 |
关键词:1; 1-二甲硫基-2-硝基乙烯; 中间体; 合成 |
中图分类号:TQ221.21 文献标识码:A 文章编号:1009-9212(2006)01-0052-03 |
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Synthesis of 1,1-bis(methylthio)-2-nitroethene |
JIA Zheng-gui(Department of chemistry; Huaiyin Teachers College; Huai'an 223301; China) |
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... |
Key words:1; 1-bis(methylthio)-2-nitroethene; intermediate product; synthesis |
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收稿日期:2005-09-26
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