3-甲基-2-丁烯-1-醇的无水酯化水解工艺研究

Anhydrous Esterification and Hydrolysis Method of Preparing 3-Methyl-2-buten-1-ol

以3-甲基-2-丁烯-1-氯为原料,开发了一种制备3-甲基-2-丁烯-1-醇的无水酯化水解工艺,利用微量水分测定仪、气相色谱、红外光谱、核磁共振对所得产物进行测试和表征。讨论了催化剂、酯化剂、反应溶剂、反应温度、反应时间和水解溶剂比例等因素对无水酯化水解工艺过程的影响,确定了最佳反应条件。在最佳反应条件下,氯代烃的酯化率>98%,酯化中间体的水解率为100%,制得的目标醇含水率<0.03%。同时,考察了水解溶液循环利用对无水酯化水解工艺过程的影响。

3-Methyl-2-buten-1-ol was prepared from isopentenyl chloride by the anhydrous esterification-hydrolysis method,and characterized by Karl fischer trace moisture meter,GC,IR and1 HNMR. The optimal conditions of the method were discussed and determined by the catalyst,the esterifying agent,the reaction solvent,the temperature,the time,the volume ratio of hydrolysis reagent and other factors. Under the best condition,the conversion of isopentenyl chloride was over 98%,the hydrolysis yield of esterification intermediate was 100%,the moisture content of the product was below 0. 03%. The effects of recycle of hydrolysis solution on the anhydrous esterification-hydrolysis method were also investigated.