HRID636648

反应详情

EQUATION

反应方程式

HRID 636648 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-methyl-5-methoxy-pyridine (2.93 g, 24 mmol) in DCM (100 mL) was added sodium sulphate (5 g, 35 mmol), followed by m-chloro-peroxy-benzoic acid (10 g, 58 mmol), and mixture was stirred at room temperature for ˜48 hours. The reaction mixture was filtered, and the white solid was washed with DCM. The filtrate was concentrated and purified by normal phase chromatography eluting with a gradient of 1:1 EtOAc/heptane to EtOAc to give 2-methyl-5-methoxy-pyridine-N-oxide (2.41 g, 72%).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. washthe white solid was washed with DCM
  3. concentrationThe filtrate was concentrated
  4. custompurified by normal phase chromatography
  5. washeluting with a gradient of 1:1 EtOAc/heptane to EtOAc