HRID1529344

反应详情

EQUATION

反应方程式

HRID 1529344 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

A solution of 5-(2-fluorophenyl)-3-iodo-1H-pyrrolo[3,2-b]pyridine (227 mg, 0.671 mmol) in THF (7 mL) was treated with TsCl (141 mg, 0.738 mmol, Fluka) and solid NaOH (32.2 mg, 0.806 mmol, VWR). The reaction was stirred at 23° C. under N2. After 45 min, the solution was diluted with EtOAc (100 ml) and washed with brine (75 mL), dried over MgSO4, concentrated in vacuo and purified by silica gel chromatography (eluent: 10-25% EtOAc/hexane), affording 5-(2-fluorophenyl)-3-iodo-1-tosyl-1H-pyrrolo[3,2-b]pyridine (238 mg, 72%). MS (ESI, pos. ion) m/z: 493.0 (M+1).

WORKUP

后处理

  1. washwashed with brine (75 mL)
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated in vacuo
  4. custompurified by silica gel chromatography (eluent: 10-25% EtOAc/hexane)