4-羟丁基缩水甘油醚的合成

摘要

以1,4-丁二醇(BDO)和环氧氯丙烷(ECH)为原料,经一步法合成了丙烯酸羟丁基缩水甘油醚中间体4-羟丁基缩水甘油醚(4-HBGE),其结构经1H NMR和MS(ESI)确证.对反应条件进行了优化,最佳反应条件为:BDO 0.1 mol,四丁基溴化铵(5 wt%)为催化剂,n(ECH)∶n(BDO)为1 ∶2, n(NaOH) ∶n(BDO)=1 ∶1.5,甲苯/水(V/V=1/1)为溶剂,于40 ℃反应6 h,经二级萃取法提纯,4-HBGE收率和纯度分别为69.5%和97.6%.%The intermediate of 4-hydroxybutyl acrylate glycidylether, 4-hydroxybutyl glycidylether(4-HBGE), was synthesized by one-step method using 1,4-butylene glycol(BDO) and epichlorohydrin(ECH) as materials.The effects of reaction conditions on the yield of 4-HBGE were investigated.The results showed that the optimum reaction conditions were as followed: BDO 0.1 mol, n(ECH) ∶n(BDO) was 1 ∶ 2, n(NaOH) ∶ n(BDO) was 1 ∶ 1.5, tetrabutylammonium bromide(5 wt%) as phase transfer catalyst and toluene/H2O(V/V=1 ∶ 1) as the solvent, reaction at 40 ℃ for 6 h, with two-step extraction, the yield and purity of 4-HBGE were 69.5% and 97.6%, respectively.