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机构地区:[1]湖北师范学院化学与环境工程学院,湖北黄石435002
出 处:《精细与专用化学品》2012年第1期36-39,共4页Fine and Specialty Chemicals
基 金:湖北省自然科学基金资助项目(2005ABA053)
摘 要:对以H_4SiW_(12)O_(40)/硅胶为催化剂,以乙酰乙酸乙酯和1,2-丙二醇为原料合成苹果酯-B的反应条件进行了研究。比较全面地研究了原料物质的量比、催化剂用量、反应时间以及带水剂用量4个因素对产品收率的影响。实验表明:H_4SiW_(12)O_(40)/硅胶是合成苹果酯-B的良好催化剂,最佳反应条件为:n(乙酰乙酸乙酯):n(1,2丙二醇)=1:1.6,催化剂用量0.30g,带水剂环己烷8mL,反应时间75min。上述条件下,苹果酯-B的收率可达89.25%。Fraistone has been synthesized by the ketalation of ethyl acetoacetate with 1,2-propanediol by using H_4SiW_(12)O_(40)/ silica gel(SG) as catalysts.The influencing factors of the synthesis were investigated.The optimum conditions were found.The optimum conditions were as follows:molar ratio of ethyl acetoacetate to 1,2-propanediol is 1:1.6,the mass of the catalyst is 0.30g(based on 0.20 mol ethyl acetoacetate),the volume of cyclohexane as the water-carrying agent is 10 mL and the reaction time is 75 min.The result shows that H_4SiW_(12)O_(40)/SG is an excellent catalyst for synthesizing fraistone and the product yield can reach 89.25%.
关 键 词:苹果酯-B H_4SiW_(12)O_(40)/硅胶 催化 缩酮反应
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