摘要
实验以丙二酸二乙酯和溴代异丁烷为起始原料,经烷基化、酯还原和醚化反应合成2,2-二异丁基-1,3-丙二醇二甲醚,分别考察了关键因素对3步合成反应的影响.适宜的工艺条件为:烷基化反应时,乙醇钠分2批加料,萃取剂为乙醚;酯还原反应时,2,2-二异丁基丙二酸二乙酯与氢化铝锂的摩尔比为1∶1.5,反应时间为60 min;醚化反应时,碘甲烷为甲基化试剂,60%氢化钠为碱,反应时间为6 h.以丙二酸二乙酯计产物的总收率为71.8%.
2,2-Diisobutyl-1,3-propanediol dimethyl ether,one kind of internal electron donors in the Ziegler-Natta catalyst,having excellent comprehensive performance was synthesized from diethyl malonate and isobutyl bromide by alkylation,ester reduction and etherification.The key effects of reaction conditions were studied and the optimal results were found as follows:in alkylation,diethyl ether as extractant and sodium ethoxide feeding in two batches;in ester reduction,molar ratio of 2,2-diisobuty diethyl malonate to LiAlH_4 1:1.5,reaction time 60 min;in etherification,iodomethane as methylation reagent,60%sodium hydride as base and reaction time 6 h.The overall yield of the desired product was 71.8%,which was about 37%higher than that reported before.The structures of the intermediates and final product were elucidated by ~1H NMR.
出处
《精细石油化工》
CAS
CSCD
北大核心
2010年第1期51-54,共4页
Speciality Petrochemicals
关键词
2
2-二异丁基-1
3-丙二醇二甲醚
烷基化
还原
醚化
合成
2,2-diisobutyl-1,3-propanediol dimethyl ether
alkylation
ester reduction
etherification
synthesis
