药用1,3-二甲基戊胺盐酸盐的合成工艺改进

Synthesis technology of 1,3-dimethyl-pentylamine hydrochloride for drug

目的合成1,3-二甲基戊胺盐酸盐并改进其工艺。方法 以乙酰乙酸乙酯和2-溴丁烷为原料,经4步合成反应得到1,3-二甲基戊胺盐酸盐,并采用单因素考察法对合成工艺进行改进。结果1,3-二甲基戊胺盐酸盐各步反应的收率均>40%,产物总收率达到12.3%。结论产物结构经1 H-NMR和13 C-NMR确认为1,3-二甲基戊胺盐酸盐。

Objective To synthesize 1, 3 dimethyl pentylamine hydroehloride and improve the synthesis. Methods We obtained 1, 3-dimethyl-pentylamine hydrochloride via 4 step reaction process from the raw material of ethyl acetoacetate and 2-butyl bromide, and synthesis was improved by single factor optimization. Results Each yield of the four reactions for 1, 3-dimethyl-pentylamine hydrochloride exceeded 40%, and the overall yield was 12.3%. Conclusion The structure of 1, 3-dimethyl-pentylamine hydrochloride is elucidated by ^1 H-NMR and ^13C-NMR.