3-氨基-1-金刚烷醇合成工艺的优化

Optimization of the preparation process of 3-amino-1-adamantane alcohol

目的制备维格列汀重要中间体3-氨基-1-金刚烷醇,并优化其制备工艺。方法以盐酸金刚烷胺为原料,用混酸反应、碱解的方法制得3-氨基1-金刚烷醇粗品,后处理过程中首次采用乙醇进行提取,并应用星点设计-效应面法优化该工艺参数。结果所制备化合物的结构经IR、1HNMR、13CNMR、MS确证;收率可达95%,纯度97.66%。结论优化后的工艺稳定、可行,具备一定实际应用价值,适合工业化生产。

OBJECTIVE To prepare the key intermediate of Vildagliptin：3 - amino - 1 adamantane alcohol and to optimize the preraration process. METHOD The crude product of 3 - amino - 1 - adamantanol was prepared by the reaction of acid and alkaline solution based on amantadine hydrochloride. The extraction process was carried out for the first time in the post - treatment process, in which the process parameters were optimized by Central composite design - response surface methodology. RESULTS The structure of the synthesized componds was confirmed by IR,1HNMR,13CNMR and MS. The yield was 95% and the purity was 97.66%. CONCLUSION The optimized process is stable and feasible, and has certain practical application value, which is suitable for indus- trial production.