HRID1376970

反应详情

EQUATION

反应方程式

HRID 1376970 的结构方程式

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

4-Hydroxy-3,5-di-tert-butylanisole (23.6 g) was dissolved in acetic anhydride (150 ml). Following the addition of conc. sulfuric acid (0.5 ml), the mixture was stirred at 70° C. for 2 h. The reaction mixture was concentrated under reduced pressure and a saturated aqueous solution of sodium hydrogen carbonate was added to the concentrate, followed by extraction with ethyl acetate. The extracted layer was dried over anhydrous magnesium acetate and concentrated. The precipitating solid was recrystallized from methanol-water (2:1) to afford 4-acetoxy-3,5-di-tert-butylanisole [24.5 g (yield, 88%)] as a white solid.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additiona saturated aqueous solution of sodium hydrogen carbonate was added to the concentrate
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialThe extracted layer was dried over anhydrous magnesium acetate
  5. concentrationconcentrated
  6. customThe precipitating solid was recrystallized from methanol-water (2:1)