HRID1177272

反应详情

EQUATION

反应方程式

HRID 1177272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
78 °C

PROCEDURE

实验过程

To a solution of 5-bromo-N,N-dimethylpyridine-2-carboxamide (730 mg, 3.19 mmol) in 10 mL of HOAc was added 1 ml of 35% H2O2. After stirring the mixture at 78° C. for 14 hours, it was cooled and concentrated under reduced pressure. The residue was made alkaline with excess solid Na2CO3 and diluted with 25 mL of CHCl3 with stirring. The inorganic salts were filtered off, and the organic layer was dried over Na2SO4. The solvent was evaporated under reduced pressure to provided the product (750 mg, 98%), which was used without further purification. MS (ESI, pos): 247.00.

WORKUP

后处理

  1. temperatureit was cooled
  2. concentrationconcentrated under reduced pressure
  3. additiondiluted with 25 mL of CHCl3
  4. stirringwith stirring
  5. filtrationThe inorganic salts were filtered off
  6. dry with materialthe organic layer was dried over Na2SO4
  7. customThe solvent was evaporated under reduced pressure