HRID912462
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
- 80 °C
PROCEDURE
实验过程
To a solution of 6-bromo-5-(2,4-difluorophenoxy)-1H-indazole (1.35 g, 4.15 mmol) and 2,2-dimethyloxirane (0.755 mL, 8.30 mmol) in DMA (20 mL) in a sealed tube was added potassium carbonate (1.72 g, 12.5 mmol), and the reaction was heated to 80° C. for 16 hours. The reaction mixture was allowed to cool to ambient temperature, diluted with ethyl acetate, and washed twice with water and once with brine. It was dried over Na2SO4, filtered, and concentrated. The residue was purified by flash chromatography on silica gel loaded and eluted with 35% ethyl acetate/hexanes to yield pure 1-(6-bromo-5-(2,4-difluorophenoxy)-1H-indazol-1-yl)-2-methylpropan-2-ol (0.60 g, 36.4% yield).
WORKUP
后处理
- temperatureto cool to ambient temperature
- washwashed twice with water and once with brine
- dry with materialIt was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by flash chromatography on silica gel
- washeluted with 35% ethyl acetate/hexanes