反应详情

温度

40 °C

To a solution consisting of 1-(2-phenoxypyrimidin-5-yl)ethanone (Step B, 400 mg, 1.87 mmol) in dichloromethane (14 mL) was added tetrabutylammonium tribromide (990 mg, 2.05 mmol). The reaction mixture was sealed with a screw top and warmed at 40° C. overnight and allowed to cool to room temperature. Hexane (4 mL) was subsequently added. After three hours and little precipitation, additional (150 mg) tetrabutylammonium tribromide was added and the reaction mixture was stirred overnight at room temperature. The pale yellow precipitate that formed was collected on a filter and washed with 1:1 dichloromethane-hexane to afford the title intermediate (375 mg, 68%); Rf 0.43 with 3:1 v/v hexanes-ethyl acetate; MS (ESI+) m/z 295, 293 (M+1, Br isotopes).

1. customThe reaction mixture was sealed with a screw top
2. temperatureto cool to room temperature
3. customlittle precipitation, additional (150 mg) tetrabutylammonium tribromide
4. additionwas added
5. customThe pale yellow precipitate that formed
6. customwas collected on
7. filtrationa filter
8. washwashed with 1:1 dichloromethane-hexane