1,8-辛二醇单边乙酰化合成工艺研究

Study of Synthesis of Monoacetate of 1,8-Octanediol

研究了1,8-辛二醇在四氢呋喃溶剂中,吡啶为缚酸剂和乙酸酐进行单边乙酰化反应制备8-乙酰氧基-1-辛醇。通过改变反应温度、反应时间、反应物配比和吡啶的用量等因素研究了1,8-辛二醇单边乙酰化的最佳制备工艺条件:溶剂为二氯甲烷、反应温度为0℃、反应时间为4.5 h、乙酸酐和1,8-辛二醇的摩尔比为0.95:1、傅酸剂吡啶的用量为乙酸酐1.2倍量(摩尔比)。在最佳工艺条件下,气相分析单边乙酰化的收率为82.7%。

8 - acetoxyo - 1 - octanol was synthesized from 1, 8 - octanediol by monoacetate reaction with acetic an-hydride using pyridine as acid binding agent in tetrahydrofuran. The influences of the reaction temperature, the reaction time, the molar ratio of acetic anhydride to 1, 8 - octanediol and the quantity of pyridine on the yield of 8 - acetoxyo - 1 -octanol were investigated. The optimum reaction conditions were reaction temperature 0 ℃, eaction time 4. 5 h, n （ acetic anhydride）/n（ 1,8 - octanediol） = 0. 95, and n （ pyridine ）/n （ acetic anhydride ） = 1.2. Under the optimum conditions, the yield of 8 - acetoxyo - 1 - octanol was 82. 7% by GC.