HRID1772606
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
- 95 °C
PROCEDURE
实验过程
To a solution of compound 10a (5.80 g, 22.6 mmol) in AcOH (20 mL), was added Br2 (7.30 g, 45.7 mmol) dropwise. The reaction mixture was stirred at 95° C. for 30 min. After cooling to rt, the product was precipitated by addition of Et2O and collected by filtration and washed with Et2O to obtain compound 10b as a yellow solid (5.50 g, 96% yield). Mass Spectrum (LCMS, ESI pos.): Calcd. for C9H8BrN3O: 254.0 (M+H). Found 254.1.
WORKUP
后处理
- temperatureAfter cooling to rt
- customthe product was precipitated by addition of Et2O
- filtrationcollected by filtration
- washwashed with Et2O