HRID2121236
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
PROCEDURE
实验过程
To a solution of the product of Example 308B (940 mg, 2.33 mmol) in ethyl acetate (50 mL) was added SnCl2.2H2O (1.85 g, 8.18 mmol) and the reaction was heated at reflux for 1 hour. The reaction mixture was cooled and basified to pH8 gradually with solid NaHCO3, stirred overnight, and extracted with ethyl acetate. The ethyl acetate extract was concentrated and the residue was purified by chromatography on silica gel (5% methanol-ethyl acetate) to give the aniline (450 mg, 52%) as an oil.
WORKUP
后处理
- temperaturethe reaction was heated
- temperatureat reflux for 1 hour
- temperatureThe reaction mixture was cooled
- extractionextracted with ethyl acetate
- extractionThe ethyl acetate extract
- concentrationwas concentrated
- customthe residue was purified by chromatography on silica gel (5% methanol-ethyl acetate)