固体光气法合成3,4-二甲氧基苯异氰酸酯

以固体光气代替光气与3,4-二甲氧基苯胺(藜芦胺)反应合成3,4-二甲氧基苯异氰酸酯,分析了影响反应的各种因素,优化后的合成条件为:以氯仿为溶剂,n(固体光气)∶n(藜芦胺)=1∶2,滴液温度0～5℃,回流温度62℃,保温时间6h。此条件下合成的产品纯度99.3%,收率82.1%。与光气法相比,该法安全方便,产品纯度和收率高。产品用红外光谱、核磁共振仪、气质联用仪进行了表征。

Synthesis of 3,4-Dimethoxyphenylisocyanate Using Triphosgene

3,4-Dimethoxyphenylisocyanate was synthesized from 3,4-dimethoxyaniline and BTC. The factors which affected the yield of the reaction were studied,and the optimized conditions in which the product was prepared in 82.1% yield with 99.3% purity was obtained as follows:chloroform as solvent,the molar ratio of BTC to 3,4-dimethoxyaniline 1∶2;titration temperature 0～5℃,the refluxing temperature 62℃,reaction time 6 h. In comparison with the phosgene method,the BTC method has advantages of good sasetey,convenient manipulation,high yield and purity. The structure of the title compound was characterized by IR,1H NMR,and GC-MS.