相转移催化合成二二茂铁丁基二硫醚

Synthesis of Diferrocenebutyl Disulfide with Phase Transfer Catalyst

采用相转移催化剂、4-氯丁基二茂铁和二硫化钠溶液反应合成了二二茂铁丁基二硫醚,考察了相转移催化剂的种类、原料摩尔比、反应温度等对反应的影响.通过正交实验法得到的最佳反应条件为:以TBAB为相转移催化剂,反应温度为45℃,三氯甲烷为溶剂,n(Na2S):n(S):n(FcCH2CH2CH2CH2Cl)=1.6:1:1,二二茂铁丁基二硫醚的产率为91.7%,而且该方法反应速度快、操作简单.通过元素分析、IR、1HNMR确定了产物的组成和结构.

Diferrocenebutyl disulfide was synthesized by the reaction of 4-chlorobutylferrocene and sodium disulfide with phase transfer catalyst （PTC）. The effect of PTC species,material mole ratio and reaction temperature on the reaction was investigated. The optimal reaction conditions obtained by orthogonal experiments are as follows： tetrabutylarnmonium bromide as PTC, chloroform as solvent,reacted at 45 C with n（Na2S） ： n（S） ： n（FcCH2CH2CHzCH2C1）=1. 6： 1：1. The isolated yield of diferrocenebutyl disulfide was 91.7%. The reaction was fast,and operable easily. The structure of diferrocenebutyl disulfide had been characterized by elemental analysis,IR and 1 HNMR.