HRID1168521
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
A mixture of diethyl 2-((2-(hydroxymethyl)-4-methylanilino)methylene)malonate (Preparation 24, 5.0 g) and acetic anhydride (5.0 mL) is heated at 130° C. for 1 h. The acetic anhydride is evaporated, and the residual solid is heated at reflux in diphenyl ether (20 ml) for 1 h. The solution is cooled and diluted with acetonitrile (5 mL) and ether (15 mL). The resulting precipitate is filtered to afford 1.8 g of the title compound.
WORKUP
后处理
- customThe acetic anhydride is evaporated
- temperaturethe residual solid is heated
- temperatureat reflux in diphenyl ether (20 ml) for 1 h
- temperatureThe solution is cooled
- additiondiluted with acetonitrile (5 mL) and ether (15 mL)
- filtrationThe resulting precipitate is filtered