乙酸-3-氯-3-甲基丁酯的合成工艺研究  

Preparation Technology of 3-Chloro-3-methyl Butyl Acetate

作　　者：曾永明[1] 魏婷[1] 何伟[1] 耿莉莉[1] 侯培桦 

机构地区：[1]昌吉学院化学与应用化学系

出　　处：《化学试剂》2018年第2期187-191,共5页Chemical Reagents

基　　金：新疆维吾尔自治区自然科学基金资助项目(2016D01C009);新疆自治区高校科研计划项目(XJEDU2017S053);昌吉学院教学研究项目(17jyyb017);国家级大学生创新创业训练计划项目(201710997005)

摘　　要：以3-甲基-3-丁烯-1-醇（MBOH）和乙酰氯为原料,经酯化、亲电加成串联反应合成了标题化合物。通过单因素实验探讨了反应温度、反应时间、配料比对产物产率的影响。在此基础上,采用响应曲面法对实验条件进行最优化选择。结果表明,合成标题化合物的最佳实验条件为n（乙酰氯）∶n（MBOH）=1.17∶1、9℃下反应230 min,在此条件下产率达95.87%。采用红外光谱、气相色谱、核磁共振光谱仪和气质联用色谱仪等对目标化合物的结构进行表征,并研究了其香气评价及稳定性研究。A simple,one-pot cascade reaction for the synthesis of 3-chloro-3-methyl butyl acetate has been developed by using MBOH and acetyl chloride as raw materials.The effect of the reaction time,temperature and feed ratio was investigated.Base on the single-factor experiments,the optimal synthetic conditions by using response surface methodology were obtained as follows：n（acetyl）∶n（MBOH）=1.17∶1 at 9℃ for 230 minute to give the target product with a maximum yield of 95.87%.The structures of the target compound were confirmed by IR,GC,GC/MS and NMR,and its aroma evaluation and stability were investigated.

关 键 词：乙酸-3-氯-3-甲基丁酯 香料 响应曲面法 合成工艺 

分 类 号：TS264.3[轻工技术与工程—发酵工程]