HRID871096

反应详情

EQUATION

反应方程式

HRID 871096 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 6-bromo-1H-pyrrolo[3,2-b]pyridine (400 mg, 2.030 mmol) and sodium hydride (60% in mineral oil) (89 mg, 2.233 mmol) in 4 mL N,N-dimethylformamide was stirred at ambient temperature for 10 minutes and 1-(bromomethyl)-3-fluorobenzene (384 mg, 2.030 mmol) was added. The mixture was heated at 100° C. for 3 hours. The mixture was cooled to ambient temperature, diluted with 100 mL of ethyl acetate and washed successively with water and brine, dried over MgSO4, filtered, and concentrated. The residue was purified by flash chromatography on Analogix IntelliFlash280 eluting with 10 to 70% ethyl acetate/hexanes to give the title compound.

WORKUP

后处理

  1. temperatureThe mixture was heated at 100° C. for 3 hours
  2. temperatureThe mixture was cooled to ambient temperature
  3. washwashed successively with water and brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified by flash chromatography on Analogix IntelliFlash280
  8. washeluting with 10 to 70% ethyl acetate/hexanes