二茂铁二羧酸双(二乙二醇)酯合成研究  

Study on synthesis of ferrocene dicarboxylic acid bis(diethylene glycol) ester

作　　者：张晓勤 常伟林 康玲 贾利亚 王建伟 Zhang Xiaoqin;Chang Weilin;Kang Ling;Jia Liya;Wang Jianwei(Liming Research & Design Institute of Chemical Industry Co.,Ltd.,Luoyang 471000,China)

机构地区：[1]黎明化工研究设计院有限责任公司

出　　处：《化学推进剂与高分子材料》2019年第5期58-62,共5页Chemical Propellants & Polymeric Materials

摘　　要：以二茂铁、乙酰氯、溴、二乙二醇等为原料,合成出中间体二乙酰二茂铁、二茂铁二羧酸、二茂铁二羧酸二甲酯,再采用酯交换工艺,通过提高二乙二醇比例,选用低毒溶剂油,并利用甲醇/溶剂油易于分层、准确控制反应终点,合成出了高质量分数的目标产物二茂铁二羧酸双(二乙二醇)酯。该方法与直接酯化法相比收率提高至80%,目标产物质量分数为93%,相比酰氯法避免了使用剧毒的草酰氯、氯化亚砜,是低成本规模化制备目标产物的优化方法。Using the ferrocene,acetyl chloride,bromine,diethylene glycol and so on as raw materials,the intermediates including diacetylferrocene,ferrocene dicarboxylic acid and ferrocene dicarboxylic acid dimethyl ester were synthesized.Then using the transesterification process,increasing the ratio of diethylene glycol,selecting the low-toxic solvent oil,utilizing the advantages of methanol/solvent oil layering easily and accurately controlling reaction end point,the target product ferrocene dicarboxylic acid bis(diethylene glycol)ester with high mass fraction was synthesized.Compared with the direct esterification method,the yield of this method increases to 80%,and mass fraction of target product is 93%.Compared with the acyl chloride method,this method avoids the use of highly toxic oxalyl chloride and sulfoxide chloride.Therefore,this method is an optimized method for large scale preparation of the target product at low cost.

关 键 词：二茂铁 二乙酰二茂铁 二茂铁二羧酸 二茂铁二羧酸二甲酯 酯交换 合成研究 

分 类 号：TQ245.2[化学工程—有机化工]