摘要
以3-羟基丁酸和乙醇为原料,在对甲苯磺酸的催化下分别以氧化钙、3A分子筛、无水硫酸镁为脱水剂,采用索氏提取器进行回流脱水合成3-羟基丁酸乙酯。对影响3-羟基丁酸乙酯收率的诸因素进行了考察。试验结果表明:加入脱水剂和带水剂可以显著提高3-羟基丁酸乙酯的收率。当原料配比为:0 1mol3-羟基丁酸、0 12mol乙醇,0 7175g对甲苯磺酸,带水剂环己烷50mL,脱水剂18 7g氧化钙,反应时间3h时,产品3-羟基丁酸乙酯的收率可达96 6%(质量分数,下同)。
Preparation of ethyl 3-hydroxybutyrate from 3-hydroxybutyric acid and ethanol was studied.Reaction was carried out in a Soxhlet extracting set,with paratoluenesulfonic acid as catalyst and CaO,molecular sieve type 3A or MgSO_4 as dehydrating agent.Various reaction parameters were also examined.Experimental results showed that the productivity of ethyl 3-hydroxybutyrate was obviously improved by adding dehydrating agent and water carrier in the reaction system.The productivity of ethyl 3-hydroxybutyrate could be attained 96.6% under the following optimum conditions:3-hydroxybutyric acid 0.1mol,ethanol 0.12mol,paratoluenesulfonic acid (0.717 5g),cyclohexane 50mL,CaO18.7g and reaction time 3h.
出处
《化学工业与工程》
CAS
2003年第6期333-336,386,共5页
Chemical Industry and Engineering
