3,3-双溴甲基氧丁环的合成

Synthesis of 3,3-Bis(bromomethyl)oxetane

以三溴新戊醇(TBNPA)为原料,在碱作用下,分别采用以乙醇作溶剂的均相法和以溴化四丁基铵作相转移催化剂的两相法(甲苯/水)合成了3,3-双溴甲基氧丁环(BBMO)。相转移催化两相合成法的收率(90.8%)明显高于均相合成法(65.6%)。在均相法中,真空蒸馏残留物为未发生反应的三溴新戊醇,约占TBNPA投料质量的20%;而在相转移催化法中,真空蒸馏残留物主要是液态低聚醚,约占TBNPA投料质量的8%。

3,3-Bis（bromomethyl） oxetane（BBMO） was synthesized from tribromoneopentyl alcohol（TBNPA） in the presence of alkali via homogeneous reaction with ethanol as solvent or phase transfer reaction with tetrabutylammonium bromide as phase transfer catalyst.The results showed that the yield of BBMO in phase transfer catalytic reaction（90.8%） was higher than that in homogeneous reaction（65.6%）.The vacuum distillation residue of homogeneous reaction was found to be unreacted TBNPA,while that of phase transfer catalytic reaction was low molecular weight polyether.