二碳酸二叔丁酯的合成工艺研究

Synthesis Research of Di-tert-butyl Dicarbonate

以三光气、叔丁醇等为原料在添加碱、相转移催化剂的条件下合成标题化合物。考察了原料物质的量比、反应温度、催化剂种类、催化剂用量、碱的类型、碱的用量等对收率的影响。结果表明,四丁基溴化铵（TBAB）为相转移催化剂,TBAB用量为NaOH量的2 wt%,反应时间2 h时,目标化合物收率最高。以三光气代替光气经相转移催化法合成目标化合物,安全高效、反应时间短、收率高。

With tert-butanol,triphosgeneand alkali as starting material,di-tert-butyl dicarbonate was prepared by phase transfer catalysis synthesis process.The effects of molar ratio of the reactants,reaction temperature,catalyst type,catalyst dosage,alkali type and alkali dosage on the reaction results were mainly investigated.When using TBAB as phase transfer catalyst,the dosage of TBAB at 2 wt% of the quality of Na OH,reaction time around 2 h,the highest yield of di-tert-butyl dicarbonate was obtained.Triphosgene instead of phosgene for phase transfer catalytic synthesis of di-tert-butyl dicarbonate was safer and more efficient,which with shorten reaction time and higher yield.