HRID333084

反应详情

EQUATION

反应方程式

HRID 333084 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

4-Bromo-2,6-dimethylpyridine (0.5 g, 2.69 mmol) was dissolved in DCM (10 ml), cooled to 0° C. and combined with a solution of m-chloroperbenzoic acid in DCM (75%, 0.928 g, 4.03 mmol in 5 ml). The resulting mixture was stirred at 0° C. for 15 minutes and for 5 hours at room temperature. The mixture was washed with saturated sodium bicarbonate solution, the phases were separated with a phase separator, the organic phase was evaporated under reduced pressure. The residue was purified by column chromatography (silica, gradient of 0.5 to 10% methanol in DCM). 475 of a yellow solid was obtained (2.35 mmol, 88%). MS (ESI) m/z=204.0 [M+1]+.

WORKUP

后处理

  1. washThe mixture was washed with saturated sodium bicarbonate solution
  2. customthe phases were separated with a phase separator
  3. customthe organic phase was evaporated under reduced pressure
  4. customThe residue was purified by column chromatography (silica, gradient of 0.5 to 10% methanol in DCM)
  5. custom475 of a yellow solid was obtained (2.35 mmol, 88%)