2,2,6,6-四甲基-3,5-庚二酮的批量制备

摘要

Using sodium hydride as condensing agent,the 2,2,6,6-tetramethyl-3 ,5-heptanedione was prepared from pinacolone and methyl pivalate. Through small experiments, the preliminary optimize reaction condition was as follows:n( PC): n(MP)-n( NaH) = 1: 1. 48: 3. 0, the dropping time of pinacolone 4 h and refluxing time 6 h. Based on those,expanded production and further optimized the reaction condition; n.(PC): n,(MP): n(NaH) =1: 1.48:1. 81,the dropping time of pinacolone 7 h,refluxing time 14 h.with yield of 82,11% ,higher than the yield reported in literature 72%.%以氢化钠为缩合剂,3,3-二甲基丁酮(PC)和二甲基丙酸甲酯(MP)为原料,制备2,2,6,6-四甲基-3,5-庚二酮.小量制备最佳条件为:n(PC):n(MP):n(NaH)=1:1.48:3.0,酮滴加时间为4h,回流时间6h.在此基础上进行扩大化生产,并对生产条件进一步优化:n(PC):n(MP):n(NaH)=1:1.48:1.81,酮滴加为7h,回流时间为14 h,产率达82.11％,高于文献报道的最高产率72％.