HRID433893

反应详情

EQUATION

反应方程式

HRID 433893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2-(4-flourophenyl)ethanesulfonyl chloride (0.7 g, 3.3 mmol) and concentrated aqueous ammonia (0.88 specific gravity, 10 ml) in ethanol (5 ml) was stirred at room temperature overnight. The reaction mixture was diluted with water (10 ml), acidified to pH 4 with citric acid (1.0 M) and then extracted with dichloromethane. The organic extracts were dried by filtering through an organic-only, permeable membrane and then concentrated under vacuum. The residue was purified by chromatography on a Biotage® Flash 40 (s) column (40 g silica) using 10-20% ethyl acetate/dichloromethane as eluant to give the title compound as an off white solid, (0.66 g).

WORKUP

后处理

  1. extractionextracted with dichloromethane
  2. customThe organic extracts were dried
  3. filtrationby filtering through an organic-only, permeable membrane
  4. concentrationconcentrated under vacuum
  5. customThe residue was purified by chromatography on a Biotage® Flash 40 (s) column (40 g silica)