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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%。
Using ethylenediamine as raw material, with acetic acid, dihalogenated two-step reaction, synthesis of 1,4-diacetyl-1,4-diazepane. The structure was characterized by IR. The effects of temperature, material ratio, time and solvent volume on the yield of the product were investigated. The optimum experimental design was optimized by orthogonal experiment, and the best method for the synthesis of 1,4 diacetyl 1,4-diazepane Process conditions: the reaction time was 10h, n (N, N’-diacetylethylenediamine): n (1,3-dichloropropane) was 1: 1.35, the reaction temperature was 65 ℃, 0.1mol N, N’-diacetyl The DMF required for ethylenediamine was 130 mL and the highest yield of the product was 57%.