论文部分内容阅读
以3,4-二甲氧基苄醇为原料,通过溴代、Arbuzov重排反应、Wittig-Horner反应和脱甲基化反应得到目标产物(E)-3,3′,4,5′-四羟基二苯乙烯,即白皮杉醇。该文考察了溴代试剂、Arbuzov重排反应温度、Wittig-Horner反应中溶剂及脱甲基反应试剂等各因素对产物产率的影响,得到最佳反应条件为:以三溴化磷为溴代试剂,Arbuzov重排反应条件为100℃反应1 h,再于120~130℃反应3~4 h,以DMF为Wittig-Horner反应溶剂,无水AlCl3作为脱甲基化试剂。通过IR、1HNMR及13CNMR确定了目标产物的结构。
Starting from 3,4-dimethoxybenzyl alcohol, the target product (E) -3,3 ’, 4,5’- Tetrahydroxystilbene, ie, Picea. In this paper, the effects of bromination reagent, Arbuzov rearrangement reaction temperature, Wittig-Horner reaction solvent and demethylation reagent on the yield of the product were investigated. The optimal reaction conditions were: phosphorous tribromide as bromine Reagents, Arbuzov rearrangement reaction conditions 100 ℃ for 1 h, and then at 120 ~ 130 ℃ for 3 ~ 4 h, DMF as Wittig-Horner reaction solvent, anhydrous AlCl3 as a demethylation reagent. The structure of the target product was confirmed by IR, 1HNMR and 13CNMR.