HRID660828
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a stirred solution of 1-benzyloxy-3-methyl-2-nitrobenzene (5.0 g, 20.6 mmol) in EtOAc (150 mL) is added SnCl2 (23.2 g, 103 mmol) and the suspension is heated at 80° C. overnight. The suspension is filtered and the filtrate washed with sat. NaHCO3 and extracted with EtOAc. The combined organic layers are washed with water, brine, then dried over MgSO4 and filtered. The solvent is removed under reduced pressure and the residue is purified by flash chromatography (hexanes/EtOAc=10:1 to 5:1) to give the title compound as a yellow oil.
WORKUP
后处理
- filtrationThe suspension is filtered
- washthe filtrate washed with sat. NaHCO3
- extractionextracted with EtOAc
- washThe combined organic layers are washed with water, brine
- dry with materialdried over MgSO4
- filtrationfiltered
- customThe solvent is removed under reduced pressure
- customthe residue is purified by flash chromatography (hexanes/EtOAc=10:1 to 5:1)