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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。
The synthesis of 1,1 ’, 3,3’-tetrakis (diphenylphosphino) ferrocene (3) was optimized. The starting material was lithium diphenylphosphine cyclopentadienide (1). Diphenylphosphinocyclopentadienyl lithium (1) is first substituted for diphenylphosphine chloride in toluene, followed by hydrogenation with n-butyllithium to give 1,3-bis (diphenylphosphino) cyclopentanebis Lithium (2) solution. The resulting solution of 2 directly reacted with ferrous chloride to give 1,1 ’, 3,3’-tetrakis (diphenylphosphino) ferrocene (3) in a total yield of 75%. Optimized process operation is simple, higher yield, suitable for industrial production.