HRID741824
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturecooled at 0° C.
- extractionThe aqueous phase was extracted 5× with ET2O
- washthe combined organic phase wash
- washwashed with brine
- dry with materialdried over MgSO4
- customevaporated
- distillationThe residue was distilled under vacuum