反应详情

Stir a mixture of 2-bromo-1-[4-(trifluoromethyl)phenyl]propan-1-one (500 g, 1.78 mol, 1 equiv), IPA (5 L), 2-aminopyrimidine (205 g, 2.13 mol, 1.2 equiv), and sodium bicarbonate (298.8 g, 3.55 mol, 2 equiv) in a thermally controlled reactor at 80° C. for 18 hours. Cool the suspension, and concentrate in vacuo. Dilute the resulting mixture with DCM (5 L), and the wash with brine (2 L). Re-extract the brine wash with DCM (2.5 L); combine all the organic extracts; dry over MgSO4; filter; collect the filtrate; and concentrate the filtrate under reduced pressure to a red gum. Slurry the resulting red gum in Et2O (1.5 L); filter; and collect the solid. Air dry the solid for 45 min to give the product as a fine off-white solid (108 g, 22% yield). ES/MS (m/z) 278 (M+1).

1. temperatureCool the suspension
2. concentrationconcentrate in vacuo
3. additionDilute the resulting mixture with DCM (5 L)
4. washthe wash with brine (2 L)
5. washRe-extract the brine wash with DCM (2.5 L)
6. dry with materialdry over MgSO4
7. filtrationfilter
8. customcollect the filtrate
9. concentrationand concentrate the filtrate under reduced pressure to a red gum
10. filtrationfilter
11. customand collect the solid
12. customAir dry the solid for 45 min