摘要
通过硝基甲烷先溴化再缩合的方法合成了2-溴-2-硝基-1,3-丙二醇,合成最佳反应条件为:在溴化反应中,NaOH与CH3NO2的物质的量比为1.1:1.0,NaOH溶液的质量浓度为25%,成盐温度为-5～0℃,溴化温度为15℃;在缩合反应中,溶液pH 5～6,缩合温度为25℃,V溶剂:V反应原料=2.0:1.0.质量分数为98%,产品总收率为83.5%.
2-Bromo-2-nitro-1,3-propanediol was synthesized by bromination of nitromethane prior to condensation.This new method used no organic solvents and the intermediate bromonitro-methane could be easily purified.Moreover,the method was beneficial for industrialization.The optimum conditions of the reaction were for bromination,the molar ratio of sodium hydroxide to nitromethane was 1.11.0,sodium hydroxide concentration was 25%,temperatures of salt forming and bromination were -50 and 15 respectively;for condensation,the pH value of the solution was 56,temperature of condensation was 25,volume ratio of solvent to raw material was 2.01.0.The overall yield of production was 83.5% with 98% purity.
出处
《化学试剂》
CAS
CSCD
北大核心
2005年第7期437-439,共3页
Chemical Reagents
