正交试验优化8-氯甲基-5,7-二羟基黄酮合成条件的研究

Study on optimized synthesis of 8-chloromethyl-5,7-dihydroxyflavone by orthogonal design

以白杨素、多聚甲醛为原料,ZnCl2为催化剂,经氯甲基化反应合成8-氯甲基-5,7-二羟基黄酮。通过单因素及正交试验研究反应温度、反应时间、催化剂用量及原料比等因素对白杨素氯甲基化反应的影响,确定了该反应的最佳条件为:反应温度为70℃,反应时间为4 h,催化剂ZnCl2与多聚甲醛的摩尔比为0.8∶1,白杨素与多聚甲醛的摩尔比为3∶1,在此条件下反应收率为59.6%。

8-chloromethyl-5,7-dihydroxyflavone was synthesized by chloromethylation of chrysin and poly-formalde- hyde with catalyst of ZnC12. The effects of the ratio of raw materials, reaction temperature and time, the amount of catalyst on the chloromethylation of chrysin were discussed by single factor test and orthogonal experiment. The optimum reaction condition is ： the reaction temperature of 70℃, reaction time of 4 h, mole ratio of ZnC12 to polyformaldehyde 0. 8 ： 1 and mole ratio of ehrysin to polyformaldehyde 4 ： 1, the yield of 8-chloromethyl-5,7-dihydroxyflavone is 59.6%.