3,3,3-三氟-2,2-二氯丙醛的合成  

Synthesis of 2,2-dichloro-3,3,3-trifluoropropanal

作　　者：袁其亮[1] 沈德隆[1] 卢鑫鑫[1] 谭成侠[1] 翁建全[1] 

机构地区：[1]浙江工业大学化学工程与材料学院,杭州310014

出　　处：《农药》2006年第7期450-451,455,共3页Agrochemicals

摘　　要：研究改进了3,3,3-三氟-2,2-二氯丙醛的合成工艺。以1,1,1-三氟三氯乙烷和三甲基氯硅烷为起始原料,首先与锌粉和N,N-二甲基甲酰胺反应生成1,1,1-三氟-2,2-二氯-3-二甲胺基-3-三甲基硅氧基丙烷,再与浓硫酸反应,得3,3,3-三氟-2,2-二氯丙醛,经精馏纯度95%以上,两步反应总收率约53.3%。中间体与产物结构经1HNMR、IR和GC-MS表征确认。Research was conducted to improve the method for synthesizing 2,2-dichloro-3,3,3-trifluoropropanal. 1,1, 1-trifluorotrichloroethane was first reacted with N,N-dimethylformamide and zinc powder to yield 2,2-dichloro-3- dimethylamino-1,1, 1-trifluoro-3-trimethylsilyloxypropane, which was next reacted with concentrated sulfuric acid to produce 2,2-dichloro-3,3,3-trifluoropropanal. Following distillation, the purity was over 95% and total yield was about 53.3%. Structures of the intermediate and target compounds were identified by ^1HNMR, IR, and GC-MS.

关 键 词：3 3 3-三氟-2 2-二氯丙醛 1 1 1-三氟-2 2-二氯-3-二甲胺基-3-三甲基硅氧基丙烷 合成 

分 类 号：TQ450.6[化学工程—农药化工]