7-hydroxy-4-methylcoumarin 1.06 g(0.006 mol) and hexamine 1.96 g (0.014 mol) were dissolved in acetic
acid (15 mL). After stirred for 7 h at 75 °C, 20% HCl (15 mL) was added into the reaction and the mixture was further heated for 45 min. After
cooled to room temperature, the reaction mixture was extracted with ether, and the combined organic layers were evaporated under reduced pressure. The residue was poured into ice water, and a pale yellow solid of 1a was obtained. Further purification was carried out by recrystallization
with hot ethanol to obtain a light yellow powder (1a).
按照一个文献上的方法合成，最初合成了两次，核磁也打出来了，后来突然出现了问题，做了几次也没想明白问题出在哪里了：1残液倒入冰水中没有沉淀析出;2有时候萃取时会出现沉淀，有那位虫友做过这个实验能详细告知一下吗？


中间体合成方法_看图王.jpg@celan@kzhch2006@liuchong630@zhulj 返回小木虫查看更多