HRID1631301

反应详情

EQUATION

反应方程式

HRID 1631301 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Bromo-5-fluoropyridin-2(1H)-one (10.0 g, 52.1 mmol) and Ag2CO3 (10.0 g, 36.5 mmol) were combined in toluene (100 mL) and iodomethane (3.89 mL, 62.5 mmol) was added drop-wise. The reaction was stirred at ambient temperature overnight, filtered through Celite and the solids were washed with toluene. The filtrate was concentrated and the residue was purified on a silica gel column (5-25% EtOAc/hexanes) to afford 3-bromo-5-fluoro-2-methoxypyridine (4.70 g, 43.8%) as a clear oil.

WORKUP

后处理

  1. filtrationfiltered through Celite
  2. washthe solids were washed with toluene
  3. concentrationThe filtrate was concentrated
  4. customthe residue was purified on a silica gel column (5-25% EtOAc/hexanes)