1,1-二氯-2-硝基乙烯的合成

以1,1,2 三氯乙烷为原料,先与氢氧化钠溶液反应,生成偏二氯乙烯,再与混酸(硝酸与盐酸)反应,得到1,1 二氯 2 硝基乙烯。考察温度、时间、三氯乙烷和氢氧化钠的用量比,偏二氯乙烯与混酸的用量比等对反应产物的影响,得到优化反应条件为:第一步反应温度65℃,反应时间1 5h,C2H3Cl3:NaOH=1 00:1 15,偏二氯乙烯的收率99%;第二步反应HNO3:HCl=1 3:1 3:1(mol/mol),反应温度20℃,反应时间3h,产物通过GC MS结构分析。

The Synthesis of 1,1-Dichloro-2-Nitroethylene

The vinylidene chloride was produced from 1,1,2-trichlorethane. The process for the production of 1,1-dichloro-2-nitroethylene which comprises reacting vinylidene chloride with nitric acid and hydrogen chloride was researched. The reaction temperature, operation time, molar ratio of 1,1,2-trichlorethane and sodium hydroxide, and molar ratio of vinylidene chloride and nitric acid, and hydrogen chloride were discussed. The optimum operation conditions were as follow: at the first step,reaction temperature 65?℃, operation time 1.5h,molar ratio of 1,1,2-trichlorethane and sodium hydroxide 1.00:1.15, The yield is 99%. At the second step,n(nitric acid)∶n(hydrogen chloride)∶n(vinylidene chloride)=1.3∶1.3∶1.0 reaction temperature 20?℃ and reaction time 3?h.The product was characterized by GC-MS.