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金刚烷甲酮(2)经高锰酸钾两步氧化制得糖尿病药物沙格列汀中间体2-(3-羟基-1-金刚烷)-2-氧代乙酸,总收率为74.7%:氧化条件①以溴化四丁铵为相转移催化剂,高锰酸钾与2投料摩尔比2.05∶1,反应温度50~55℃、pH12~13;②续加1.2当量的高锰酸钾,温度40~45℃,pH 8~9。
Adamantane methanone (2) Oxalic acid saxagliptin intermediate 2- (3-hydroxy-1 -adamantane) -2-oxoacetic acid was obtained by two steps oxidation of potassium permanganate with the total yield of 74.7% : Oxidation conditions ① tetrabutylammonium bromide as phase transfer catalyst, potassium permanganate and 2 feeding molar ratio of 2.05: 1, the reaction temperature is 50 ~ 55 ℃, pH 12 ~ 13; ② continued to add 1.2 equivalents of potassium permanganate, Temperature 40 ~ 45 ℃, pH 8 ~ 9.