HRID1258555

反应详情

EQUATION

反应方程式

HRID 1258555 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 6-bromo-3-fluoro-2-methylpyridine (2.84 g, 14.94 mmol, 1 eq.) was dissolved in DCM (250 ml) and cooled to 0° C. Then mCPBA (7.34 g, 29.89 mmol, 2 eq.) was added by portions and the reaction was warmed to r.t. and stirred for 48 h. A sat. aqueous solution of NaHCO3/Na2S2O3 (1/1) was added and stirring allowed for 5 min. Then DCM was added and the layers separated. The aqueous layer was extracted with DCM then the organics were combined, dried over MgSO4 and concentrated. 6-bromo-3-fluoro-2-methylpyridine 1-oxide (2.94 g, 89%) was obtained as a white solid.

WORKUP

后处理

  1. temperaturethe reaction was warmed to r.t.
  2. stirringstirring
  3. waitallowed for 5 min
  4. customthe layers separated
  5. extractionThe aqueous layer was extracted with DCM
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated