HRID2196666

反应详情

EQUATION

反应方程式

HRID 2196666 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Iodo-1H-pyrrolo[2,3-b]pyridine (4.55 g, 18.7 mmol) and K2CO3 (7.73 g, 55.9 mmol) were dissolved in acetonitrile (200 mL). Benzenesulfonyl chloride (4.76 mL, 37.3 mmol) was added, and the reaction mixture was heated to reflux for 10 hours. The reaction mixture was cooled and partitioned between EtOAc and water. The organic layer was washed with water (2×), brine, and dried over Na2SO4 and concentrated. The resulting residue was purified by column chromatography (4:1 to 0:1 hexane/DCM) giving 3-iodo-1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridine (5.31 g, 74.1%).

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 10 hours
  3. temperatureThe reaction mixture was cooled
  4. custompartitioned between EtOAc and water
  5. washThe organic layer was washed with water (2×), brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated
  8. customThe resulting residue was purified by column chromatography (4:1 to 0:1 hexane/DCM)