| 脱水法合成3-羟基丁酸乙酯 |
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| 引用本文： | 王彦飞,马沛生,王加宁,夏淑倩.脱水法合成3-羟基丁酸乙酯[J].化学工业与工程,2003,20(6):333-336,386. |
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| 作者姓名： | 王彦飞 马沛生 王加宁 夏淑倩 |
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| 作者单位： | 天津大学化工学院一碳化工国家重点实验室,天津,300072 |
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| 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：0．1mol 3-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)。
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| 关 键 词： | 3-羟基丁酸乙酯 脱水法 酯化反应 带水剂 脱水剂 乙醇 甲苯磺酸 |
| 文章编号： | 1004-9533(2003)06-0333-04 |
Synthesis of Ethyl 3-hydroxybutyrate by Dehydration |
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| WANG Yan-fei,MA Pei-sheng,WANG Jia-ning,XIA Shu-qiancal Engineering,Tianjin University,Tianjin ,China.Synthesis of Ethyl 3-hydroxybutyrate by Dehydration[J].Chemical Industry and Engineering,2003,20(6):333-336,386. |
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| Authors: | WANG Yan-fei MA Pei-sheng WANG Jia-ning XIA Shu-qiancal Engineering Tianjin University Tianjin China |
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| Affiliation: | WANG Yan-fei,MA Pei-sheng,WANG Jia-ning,XIA Shu-qiancal Engineering,Tianjin University,Tianjin 300072,China) |
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| Abstract: | 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. |
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| Keywords: | ethyl 3-hydroxybutyrate dehydration esterfication water carrier dehydrating agent |
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