HRID845369

反应详情

EQUATION

反应方程式

HRID 845369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the aniline from (c) (19.8 g, 44.2 mmole) and the β-ketoester from (e) (13.0 g, 44.2 mmole) in xylene (160 ml) were heated under reflux, using a Dean & Stark apparatus, for 5 hours. Over the final hour, the volume of the mixture was reduced to 75 ml by distillation. 60-80 petroleum ether (300 ml) was added with cooling and the solid collected by filtration. The product was isolated as a brown solid (24.2 g, 82%). m.p. 94-96%.

WORKUP

后处理

  1. temperatureunder reflux
  2. distillationOver the final hour, the volume of the mixture was reduced to 75 ml by distillation
  3. addition60-80 petroleum ether (300 ml) was added
  4. temperaturewith cooling
  5. filtrationthe solid collected by filtration