HRID4382

反应详情

EQUATION

反应方程式

HRID 4382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1,3-Cyclohexanedione (3.1 g) and the product of Stage (i) (5.6 g) in ethanol (196 ml) and water (39 ml) was stirred at room temperature for 3 h and then heated to reflux for 14 h. The resulting solution was allowed to cool, poured into water (500 ml) and the precipitate filtered and washed with isopropyl acetate and ether to give a solid. Recrystallisation from methanol gave the title compound as a solid (2.5 g) m.p. 235°-237°.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 14 h
  3. temperatureto cool
  4. filtrationthe precipitate filtered
  5. washwashed with isopropyl acetate and ether
  6. customto give a solid
  7. customRecrystallisation from methanol