HRID339507

反应详情

EQUATION

反应方程式

HRID 339507 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 2-methoxy-5-trifluoromethoxybenzaldehyde (2.0 g, 9.09 mmol) and 50% KOH (4.1 ml) in MeOH (15 ml) at 65° C. was added dropwise hydrogen peroxide (30%, 7.4 ml) over 20 min. The reaction mixture was then stirred at 65° C. for 10 min., cooled to room temperature, acidified with 1 M HCl, and extracted with Et2O (3×40 ml). The combined organic extracts were washed with brine (35 ml), dried (Na2SO4) and the solvent removed under reduced pressure to give a pale yellow viscous oil which solidified at room temperature overnight to give the title compound (1.95 g, 91%) as a pale yellow solid.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. extractionextracted with Et2O (3×40 ml)
  3. washThe combined organic extracts were washed with brine (35 ml)
  4. dry with materialdried (Na2SO4)
  5. customthe solvent removed under reduced pressure
  6. customto give a pale yellow viscous oil which
  7. waitsolidified at room temperature overnight