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1-金刚烷甲酸经混酸氧化得3-羟基-1-金刚烷甲酸,经酰氯化、丙二酸二乙酯取代、硫酸/冰醋酸脱羧及羟基化,“一锅法”制得3-羟基-1-金刚烷甲基酮,经高锰酸钾氧化得沙格列汀关键中间体2-(3-羟基-1-金刚烷基)-2-氧代乙酸。本研究还对“一锅法”的具体过程分步研究并进行结构确证。优化过的路线试剂价廉易得,条件温和,操作简便易控,总收率约61%(以1-金刚烷甲酸计)。
1-adamantanecarboxylic acid by mixed acid oxidation of 3-hydroxy-1-adamantane carboxylic acid, acid chloride, diethyl malonate, sulfuric acid / acetic acid decarboxylation and hydroxylation -hydroxy-1-adamantane methyl ketone and oxidized by potassium permanganate to give 2- (3-hydroxy-1 -adamantyl) -2-oxoacetic acid as the key intermediate of saxagliptin. This research also makes a step-by-step study on the specific process of “one-pot method” and confirms its structure. Optimized routes Reagents cheap and easy, mild conditions, easy to operate and easy to control, the total yield of about 61% (1-adamantane formic acid dollars).