HRID49602

反应详情

EQUATION

反应方程式

HRID 49602 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under an argon atmosphere, a mixture of 3-bromo-2-hydroxypyridine (3.49 g, 20 mmol), silver carbonate (3.67 g, 13.31 mmol), and iodomethane (1.5 mL, 24.1 mmol) in benzene (30 mL) was stirred in the dark at 40° C. to 50° C. for 24 hours, cooled in an ice bath, and filtered. The filtrate was washed once with 2% aqueous sodium bicarbonate and twice with water, dried (MgSO4), the benzene was evaporated at atmospheric pressure, and the residue was purified by flash chromatography (eluting with hexane/ethyl acetate, 2:1) to 10 obtain the title compound (2.35 g, 12.5 mmol, 62%).

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. filtrationfiltered
  3. washThe filtrate was washed once with 2% aqueous sodium bicarbonate and twice with water
  4. dry with materialdried (MgSO4)
  5. customthe benzene was evaporated at atmospheric pressure
  6. customthe residue was purified by flash chromatography (eluting with hexane/ethyl acetate, 2:1) to 10