HRID595175

反应详情

EQUATION

反应方程式

HRID 595175 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2,6-Dibromopyridin-4-amine, DMAP (0.048 g, 0.397 mmol) and pyridine (0.48 ml, 5.95 mmol) were taken-up in THF (7.9 ml) under argon. Acetic anhydride (0.41 ml, 4.37 mmol) was slowly added and the mixture was stirred overnight at room temperature. The reaction was then heated to 65° C. for 5 days and cooled to room temperature, diluted with methanol, and concentrated under reduced pressure. The residue was purified by chromatography on silica gel (0-100% EtOAc/hexanes) to afford N-(2,6-dibromopyridin-4-yl)acetamide as a light yellow solid. MS ESI calc'd. for C7H6Br2N2O [M+H]+ 294. found 294.

WORKUP

后处理

  1. temperatureThe reaction was then heated to 65° C. for 5 days
  2. temperaturecooled to room temperature
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by chromatography on silica gel (0-100% EtOAc/hexanes)