过渡金属催化的偕二卤代烯烃的制备方法优化探索

Exploration of the Preparation Method Optimization of Bisphosphonate Bromine Rubber Catalyzed by Transition Metal

本实验以苯甲醛为原料,在干燥的二氯甲烷溶液中,与四溴化碳(CBr_4)和三苯基膦(PPh_3)发生叶立德反应,制备出原料偕二卤代烯烃;实验发现采用价格低廉、经济环保的过渡金属铜(CuI)作为催化剂,以TMEDA作为配体,以K_2CO_3为傅酸剂,以为反应溶剂,以(2,2-二溴乙烯基)苯和咪唑化合物的偶联反应为研究对象,在80℃下顺利反应生成偶联产物;该探索条件操作简单,并降低三苯基膦的用量,同时减小对环境的污染,其底物使用范围广泛,目标产物选择性好,得到中等偏高的产率。

This experiment takes benzaldehyde as raw materials, under the condition of dry dichloromethane solution, make the raw meterials react with rbon tetrabromide(CBr4) and triphenylphosphine(PPh3) to prepare the raw material of bisphosphonate bromine rubber; Through the experiment, we found that adopting the low price of and economic environment of transitional metallic copper(CuI) as catalyst, taking the TMEDA as the ligand, the K2CO3 as the acid agent, the dioxane as the reaction solvent and the coupled reaction of (2,2 - dibromo vinyl) benzene and imidazole derivate as the research object, besides, in the condition of 80a??, successfully get reaction and generate into coupled product. This exploration condition is easy to operate and reduces the dosage of Smooth reaction under coupling products; The exploration conditions of the operation is simple, and reduce the dosage of triphenylphosphine, meanwhile, it reduces the pollution to the environment, besides, the range of the used substrate is wide, the targeted products have a good selectivity, finally get a medium or higher level of productive rate.