HRID602379

反应详情

EQUATION

反应方程式

HRID 602379 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

5-Bromo-2-fluoro-4-methoxybenzaldehyde (1 g, 4.3 mmol), p-toluenesulfonic acid monohydrate (163 mg, 0.86 mmol) and trimethyl orthoformate (2.4 mL, 21 mmol) were dissolved in methanol (20 mL) and stirred under heating and reflux for 1 hour. After standing to cool the reaction mixture, triethylamine (2 mL) was added thereto and further stirred for 10 minutes. The mixture was added with saturated brine and ethyl acetate, and the organic layer was separated, followed by washing with saturated brine. The organic layer was dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure to obtain 5-bromo-2-fluoro-4-methoxybenzaldehyde dimethylacetal (1.19 g, 100%).

WORKUP

后处理

  1. temperatureunder heating
  2. temperaturereflux for 1 hour
  3. additionwas added
  4. stirringfurther stirred for 10 minutes
  5. customthe organic layer was separated
  6. washby washing with saturated brine
  7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  8. customthe solvent was evaporated under reduced pressure