一锅法合成3,6-二氯-4-碘哒嗪

Synthesis of 3,6-dichloro-4-idopyridazine

以3,6-二氯哒嗪为原料,在四甲基哌啶氯化锌氯化锂(TMPZnCl·LiCl)作用下发生锂化反应,所得3,6-二氯哒嗪-4-基锂和单质碘进行碘化反应"一锅法"合成3,6-二氯-4-碘哒嗪,并采用1H-NMR和ESI-MS对目标产物的结构进行了表征。对碘取代反应的因素进行了考察,得到的最佳反应条件为:物料比n(I2)∶n(3,6-二氯哒嗪)=1.5∶1,反应温度为25℃,反应时间为30min。在此最佳反应条件下,3,6-二氯-4-碘哒嗪的收率为85.0%。

3,6-Dichloro-4-iodopyridazine was synthesized from 3,6-dichloropyridazine as starting material through a two-step reaction including lithiation reaction with TMPZnCl·LiCl and iodination reaction in a one pot process.The structure of the product was characterized by 1H-NMR and MS.The optimal iodination reaction conditions were as follows,n(I2)∶n(3,6-dichloropyridazine)=1.5∶1;the reaction was stirred at 25℃for 30 min,the target compound was obtained in a yield of 85.0%.