4-羟丁基缩水甘油醚的合成

Synthesis of 4-Hydroxybutyl Glycidylether

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 glyeidylether（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/H20（ 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.