HRID37857

反应详情

EQUATION

反应方程式

HRID 37857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Hydrogen peroxide (30%, 1.76 mL, 17.4 mmol) was added to a solution of 2-bromo-6-methyl-pyridine (1.0 g, 5.80 mmol) in acetic acid (20 mL), and heated for 24 h at 90° C. The reaction mixture was cooled to ambient temperature, and partitioned between dichloromethane and water. The aqueous phase was separated and extracted with dichloromethane. The combined organic phases were washed thoroughly with water and dried over anhydrous sodium sulfate. Concentration in vacuo afforded 2-bromo-6-methyl-pyridine 1-oxide (820 mg, 75%) as a brown liquid which was used in the next step without further purification.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to ambient temperature
  2. custompartitioned between dichloromethane and water
  3. customThe aqueous phase was separated
  4. extractionextracted with dichloromethane
  5. washThe combined organic phases were washed thoroughly with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationConcentration in vacuo