1,4-二乙酰基-1,4-二氮杂环庚烷合成工艺的研究

Study on synthesis of 1,4-diacetyl-1,4-diazacycloheptane

采用乙二胺为原料,与乙酸、二卤代烷经两步反应,合成出1,4-二乙酰基-1,4-二氮杂环庚烷。并通过IR进行了结构表征。考察了温度、物料配比、时间、溶剂体积等对产品收率的影响,并采用正交实验优化实验设计,最终确定合成1,4二乙酰基1,4二氮杂环庚烷的最佳工艺条件:反应时间10h,n(N,N'-二乙酰乙二胺):n(1,3二氯丙烷)为1:1.35,反应温度为65℃,溶解0.1mol N,N'二乙酰乙二胺所需DMF为1 30mL,产品的收率最高为57%。

1,4-Diacetyl-1,4-diazacycloheptane was synthesized with 1,2-ethylenediamine.acetic acid and 1,3-dichloropropane as raw materials.Through single-factor and orthogonal experiments,the influencing factors of the synthetic process were researched,the optimum conditions of preparing 1,4-diacetyl-1,4-diazacycloheptane were as follows：the reaction time is 10h,the reaction temperature is 65℃,the molar ratio of N,N＇-diacetylethylenediamine and 1,3-dichloropropane is 1：1,35 and the volume of DMF is 130mL.Under the above conditions, the highest yield of 1,4-diacetyl-1,4-diazacycloheptane achieved 57%.