双环3.2.1辛烷-2,4-二酮的改进合成

摘要

以2-降莰烷酮为起始原料,通过Mannich反应、Baeyer-Villiger反应和缩合反应制得双环[3.2.1]辛烷-2,4-二酮.在Mannich反应中,采用水蒸汽蒸馏有利于产品的分离提纯、促进中间产物转化为最终产物,达到了反应分离的效果;在Baeyer-Villiger反应中,通过改变甲醇和双氧水的加料顺序可避免过度氧化,提高产品收率.优化条件下产品的总收率为61.5%.%Bicyclo[3.2.1]octane-2,4-dione was synthesized using 2-norbornanone via Mannich reaction, Baeyer-Villiger reaction and self-condensation reaction. Steam distillation is used in Mannich reaction for product separation and to facilitate the transformation of intermediates into product, which combines reaction and separation together. Moreover, variation of addition sequence of methanol and hydrogen peroxide in Baeyer-Villiger reaction can improve product yields by avoiding excessive oxidation. The total yield of the final product is 61.5% under optimized conditions.