HRID1687

反应详情

EQUATION

反应方程式

HRID 1687 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

The 2-ethyl-3-chloromethylpyridine (2.4 g, 15.4 mmol) was dissolved in CHCl3 (100 mL) and cooled under nitrogen to 0° C. and m-chloroperbenzoic acid (55%, 4.2 g) was added in small portions. The reaction was stirred for 2 hours. The reaction was extracted twice with saturated aqueous sodium bicarbonate (100 mL). The organic phase was dried with MgSO4, filtered and the solvent was removed under reduced pressure. The residue was chromatographed on silica gel packed in 98:2 CH2Cl2 :MeOH and eluted with the same. The appropriate fractions were combined and the solvent removed under reduced pressure the give the desired 2-ethyl-3-chloromethylpyridine-N-oxide.

WORKUP

后处理

  1. extractionThe reaction was extracted twice with saturated aqueous sodium bicarbonate (100 mL)
  2. dry with materialThe organic phase was dried with MgSO4
  3. filtrationfiltered
  4. customthe solvent was removed under reduced pressure
  5. customThe residue was chromatographed on silica gel
  6. washMeOH and eluted with the same
  7. customthe solvent removed under reduced pressure the