反应详情

温度

90 °C

To a solution of compound 287 (14 g, 1 eq.) in EtOH (140 mL) was added 3-bromo-1,1,1-trifluoroacetone (8.8 mL, 1.2 eq.). The mixture was stirred at 90° C. for 16 hrs and concentrated in vacuo. DCM (20 mL) and water (20 mL) were added. Organics were dried over Na2SO4, filtered, concentrated under reduced pressure, and flushed on a silica gel column with 5% MeOH/DCM to yield compound 288 as a beige compound in 12% yield. MS (ESI, EI+): m/z=292 (MH+).

1. concentrationconcentrated in vacuo
2. additionDCM (20 mL) and water (20 mL) were added
3. dry with materialOrganics were dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customflushed on a silica gel column with 5% MeOH/DCM