HRID651645

反应详情

EQUATION

反应方程式

HRID 651645 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Benzenesulfonyl chloride (3 mL, 23.5 mmol) is added dropwise to a solution of tetrabutylammonium hydrogen sulfate (0.53 g, 1.56 mmol), sodium hydroxide (1.56 g, 38.9 mmol) and 4-chloro-1H-pyrrolo[3,2-c]pyridine (2.38 g, 15.6 mmol) (prepared according to Rasmussen, M. J. Het. Chem, 1992, 29, 359) in CH2Cl2. The mixture is stirred at room temperature for 4 hours the diluted with CH2Cl2 and washed with saturated NH4Cl solution and brine. The organic layer is dried over MgSO4, filtered and concentrated. The crude product is purified by column chromatography eluting with 1% MeOH/CH2Cl2 to 2% MeOH/CH2Cl2 to afford the title product (3.21 g, 11 mmol) as a white solid.

WORKUP

后处理

  1. washwashed with saturated NH4Cl solution and brine
  2. dry with materialThe organic layer is dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude product is purified by column chromatography
  6. washeluting with 1% MeOH/CH2Cl2 to 2% MeOH/CH2Cl2