HRID2121236

反应详情

EQUATION

反应方程式

HRID 2121236 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe reaction was heated
  2. temperatureat reflux for 1 hour
  3. temperatureThe reaction mixture was cooled
  4. extractionextracted with ethyl acetate
  5. extractionThe ethyl acetate extract
  6. concentrationwas concentrated
  7. customthe residue was purified by chromatography on silica gel (5% methanol-ethyl acetate)