HRID260438

反应详情

EQUATION

反应方程式

HRID 260438 的结构方程式

CONDITIONS

反应条件

温度
165 °C

PROCEDURE

实验过程

To 50 g (0.33 mol) of 3-acetoxytoluene from Step 1 was added AlCl3 (60 g, 0.45 mol) and the resulting mixture was heated at 165° C. for 20 min., then cooled at 0° C. and HCl 1N was carefully added followed by Et2O. The aqueous phase was extracted 5× with Et2O and the combined organic phase wash washed with brine, dried over MgSO4 and evaporated. The residue was distilled under vacuum to give 42.2 (84%.) of the title compound.

WORKUP

后处理

  1. temperaturecooled at 0° C.
  2. extractionThe aqueous phase was extracted 5× with Et2O
  3. washthe combined organic phase wash
  4. washwashed with brine
  5. dry with materialdried over MgSO4
  6. customevaporated
  7. distillationThe residue was distilled under vacuum