全氟丁酸还原制备七氟丁醇的工艺  

Preparation of 1,1-dihydroperfluorobutanol by reducing methyl heptafluorobutyrate

作　　者：奚强[1] 胡杨[1] 张志鹏[1] 杨海涛[1] 舒畅[1] 曾天宇 

机构地区：[1]武汉工程大学化学与环境工程学院,湖北武汉430074

出　　处：《武汉工程大学学报》2015年第3期5-8,共4页Journal of Wuhan Institute of Technology

摘　　要：针对七氟丁醇合成工艺复杂,产率低下的问题,以全氟丁酸、甲醇作为起始原料,对甲基苯磺酸为催化剂,合成全氟丁酸甲酯,然后以硼氢化钠还原全氟丁酸甲酯,得到七氟丁醇.结果显示:对于全氟丁酸甲酯的合成反应,当醇酸摩尔比为2∶1、催化剂用量为原料酸质量的0.6%,反应时间为3 h时,全氟丁酸的转化率达到85%,酯的粗品经蒸馏和水洗后即可用于还原反应;对于还原反应,当还原剂和酯的摩尔比为0.8,反应温度处于30℃,其还原效果最佳.优化后全氟丁醇的总收率可达到77.35%,目标产物经由核磁氢谱、碳谱和氟谱表征.该反应条件相对温和,原料常见且容易得到,适合工业化大规模生产.Aimed at complicated synthesis processes, low production rate of preparing 1,1-dihydroperfluorobutanol, heptafluorobutyric and methyl alcohol were applied as starting materials to prepare 1,1-dihydroperfluorobutanol. Via esterification with 4-toluene sulfonic acid as catalyst and reduction with sodium borohydride as reductant,1,1-dihydroperfluorobutanol was carried out. The results show that the yield of esterification reaction is 85% when the molar ratio of heptafluorobutyric to methyl alcohol is 2∶1, the mass ratio of catalyst to 4-toluene sulfonic acid is 0.6% and the refluxing time is 3 h; the optimal condition of reduction reaction is demonstrated when the reaction temperature is 30 ℃ and the molar ratio of reductant to ester is 0.8.The total yield is 77.35%, and the target product has characterized by nuclear magnetic resonance spectrum spectroscopy. This method is suitable for industry with mild conditions and low cost.

关 键 词：七氟丁醇 全氟丁酸甲酯 全氟丁酸 

分 类 号：TQ222.2[化学工程—有机化工]