摘要
以氢溴酸和饱和溴水为溴化试剂,与乙酰基二茂铁反应合成了溴乙酰基二茂铁。目标化合物的结构经IR及1 H NMR确证。讨论了反应温度,氢溴酸用量、饱和溴水滴加速率对收率的影响,并通过单因素讨论和正交实验确定最佳反应条件为:反应温度0℃,HBr用量1.5mL(25mmol乙酰基二茂铁),饱和溴水的滴加时间2h。在最优条件下重复实验收率可达79.6%。与传统的合成工艺相比,以饱和溴水作为酰化试剂反应过程易控制,操作简便,成本低,反应时间短,后处理简单。
Bromoacetylferrocene was prepared from acetylferrocene, with hydrogen bromide acid and saturated bromine as bromide reagent. The structure of Bromoacetylferrocene was characterized by IR and 1 H NMR. The effect of temperature, dosage of hydrogen bromideacid and adding rate of saturated bromine water on the yield was discussed. Optimum synthetic condition was informed by the single factor discussion and orthogonal experiment： the reaction temperature was 0℃, dosage of hydrogen bromide was 1.5 mL （25mmol acetylferrocene） and adding times of saturated bromine water was 2 h. Yield could achieve 79.6% under this condition. Compared with the traditional synthesis process, advantages as easy to control, lower cost, shorter reaction time, simple treatment and higher yield is obvious with hydrogen bromide as bromide reagent.
出处
《精细石油化工》
CAS
CSCD
北大核心
2015年第4期32-35,共4页
Speciality Petrochemicals
基金
陕西省教育厅重点实验室项目(13J017)
973计划前期研究专项(2014CB260411)
关键词
溴乙酰基二茂铁
合成
氢溴酸
饱和溴水
bromoacetylferrocene
synthesis
hydrogen bromide acid
saturated bromine water
