HRID711363

反应详情

EQUATION

反应方程式

HRID 711363 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To the suspension of 7-bromoquinoxalin-2-ol (2 g, 8.88 mmol) in neat phosphorus oxychloride (7 mL) was added DMF (2 drops). The mixture was heated to 100° C. for 3 h. Then it was cooled to room temperature. Phosphorus oxychloride was removed under vacuum, and the residue was dissolved into EtOAc and dropped into ice water with stirring. The mixture was extracted with EtOAc for three times, the combined organic layer was washed with saturated NaHCO3 solution. Then the organic layer was concentrated to afford 7-bromo-2-chloroquinoxaline as a solid in 93% yield (2 g).

WORKUP

后处理

  1. temperatureThen it was cooled to room temperature
  2. customPhosphorus oxychloride was removed under vacuum
  3. dissolutionthe residue was dissolved into EtOAc
  4. additiondropped into ice water
  5. extractionThe mixture was extracted with EtOAc for three times
  6. washthe combined organic layer was washed with saturated NaHCO3 solution
  7. concentrationThen the organic layer was concentrated