HRID1168521

反应详情

EQUATION

反应方程式

HRID 1168521 的结构方程式

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

  1. customThe acetic anhydride is evaporated
  2. temperaturethe residual solid is heated
  3. temperatureat reflux in diphenyl ether (20 ml) for 1 h
  4. temperatureThe solution is cooled
  5. additiondiluted with acetonitrile (5 mL) and ether (15 mL)
  6. filtrationThe resulting precipitate is filtered