HRID339511

反应详情

EQUATION

反应方程式

HRID 339511 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a stirred solution of 50% w/v KOH (0.8 ml) and 4-(3,3,3-trifluoropropoxy)benzaldehyde (0.4 g, 1.83 mmol) in MeOH (4 ml) at 65° C. was added dropwise over 20 min aqueous hydrogen peroxide (30 wt. % in water, 1.5 ml). On completion of the addition the reaction mixture was heated at 65° C. for a further 10 min. On cooling to room temperature, the reaction mixture was acidified with 1 M HCl and extracted with Et2O (3×25 ml). The combined organic extracts were washed with brine (25 ml), dried (Na2SO4) and the solvent removed under reduced pressure to give the title compound (0.36 g, 83%) as a colourless solid which was used without further purification.

WORKUP

后处理

  1. customat 65° C.
  2. additionOn completion of the addition the reaction mixture
  3. temperatureOn cooling to room temperature
  4. extractionextracted with Et2O (3×25 ml)
  5. washThe combined organic extracts were washed with brine (25 ml)
  6. dry with materialdried (Na2SO4)
  7. customthe solvent removed under reduced pressure