HRID711363
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThen it was cooled to room temperature
- customPhosphorus oxychloride was removed under vacuum
- dissolutionthe residue was dissolved into EtOAc
- additiondropped into ice water
- extractionThe mixture was extracted with EtOAc for three times
- washthe combined organic layer was washed with saturated NaHCO3 solution
- concentrationThen the organic layer was concentrated