HRID14492

反应详情

EQUATION

反应方程式

HRID 14492 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

7,8-Diamino-3-(4-chlorophenyl)-2-isopropyl-chromen-4-one (80 mg, 0.243 mmol) is dissolved in trifluoroacetic acid (1.4 ml), dilute hydrochloric acid (2M, 0.1 ml) is added, and the mixture is heated at 110° C. for 2.5 h. The reaction mixture is cooled to room temperature, diluted with ethyl acetate (50 ml) and washed with saturated sodium bicarbonate solution (2×40 ml), water (40 ml) and saturated brine (40 ml). The organic layer is dried (MgSO4), filtered and evaporated to give a solid. This is triturated with dichloromethane containing a few drops of ethyl acetate and filtered to give a colourless powder.

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled to room temperature
  2. washwashed with saturated sodium bicarbonate solution (2×40 ml), water (40 ml) and saturated brine (40 ml)
  3. dry with materialThe organic layer is dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated
  6. customto give a solid
  7. customThis is triturated with dichloromethane containing a few drops of ethyl acetate
  8. filtrationfiltered
  9. customto give a colourless powder