Tert-Alkyl chlorides 5 are prepared in good yield from the corresponding alcohols 1 in a facile two step synthesis. The method involves treatment of the corresponding crude oxalyl monochloride alkyl ester 2 with N-hydroxy-pyridine-2-thione sodium salt 3 in tetrachloromethane at reflux to give the bright yellow N-(alkoxyoxalyloxy) pyridine-2-thiones 4 which undergo decomposition to the chlorides 5 in good yield. The reaction is conveniently monitored by the loss of colour from the mixed anhydride.
通过简单的两步合成法,可以从相应的醇 1 中制备出产率很高的叔烷基
氯化物 5。该方法包括在四
氯甲烷中用 N-
羟基吡啶-2-
硫酮钠盐 3 在回流条件下处理相应的粗
草酸单
氯烷基酯 2,得到亮黄色的 N-(烷氧基氧涟氧基)
吡啶-2-
硫酮 4,然后分解成
氯化物 5,收率很高。通过混合酸酐的失色可以很方便地监测反应。