摘要
优化了1,1',3,3'-四(二苯膦基)二茂铁(3)的合成工艺,起始原料为二苯膦基环戊二烯锂(1)。二苯膦基环戊二烯锂(1)先与二苯基氯化磷在甲苯中发生取代反应,继而用正丁基锂拔氢得到1,3-双(二苯膦基)环戊二烯锂(2)的溶液。所得2的溶液直接与氯化亚铁回流反应得到1,1',3,3'-四(二苯膦基)二茂铁(3),总收率75%。优化后的工艺操作简便,收率更高,适合工业化生产。
This manuscript describes an optimized process for the synthesis of 1, 1＇, 3, 3＇ - tetrakis （diphenylphosphino） - ferrocene （3） using diphenylphosphinocyclopentadienyllithium （1） as starting material, which firstly reacted with chlorodiphenylphosphine via substitution reaction in toluene and then n - BuLi to give the solution of 1, 3 - diphenylphosphinocyclopentadienyllithium （2） which could be used in the subsequent reaction without further purification. The solution of I, 3 - diphenylphosphinocyclopentadienyllithium （2） reacted with iron dichloride under refluxing at 85 ℃ leading to 1, 1＇, 3, 3＇ - tetrakis （diphenylphosphino） - ferrocene （3） in 75% yieldo The optimized process is simpler, higher yielding and suitable for industrial production.
作者
马金焕
Ma Jinhuan(Lunan Pharmaceutical Group, National Engineering and Technology Research Center of Chirality Pharmaceutical, Linyi 276006, Chin)
出处
《山东化工》
CAS
2017年第7期18-19,共2页
Shandong Chemical Industry
