HRID1159763

反应详情

EQUATION

反应方程式

HRID 1159763 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Aq. 2.5 M NaOH (5 mL) was added to a stirring mixture of 4-bromo-1H-indole (1000 mg, 5.3 mmol), 2-methylbenzenesulfonyl chloride (1100 mg, 5.6 mmol) and tetrabutylammonium hydrogen sulfate (173 mg, 0.5 mmol) in DCM (10 mL). The reaction mixture was stirred at ambient temperature overnight. The mixture was diluted with DCM and water and the layers were separated. DCM was washed with water 2 times, dried (MgSO2) and concentrated to give 1.6 g of crude material that was purified using flash chromatography (SiO2, eluent EtOAc:hexane 9:1) giving the title product (1 g, 54%). MS (ESI+) for C15H12BrNO2S m/z 350 (M+H)+.

WORKUP

后处理

  1. customthe layers were separated
  2. washDCM was washed with water 2 times
  3. dry with materialdried (MgSO2)
  4. concentrationconcentrated
  5. customto give 1.6 g of crude material that
  6. customwas purified