反应详情

To a solution of 5-bromo-N,N-diethyl-2-(2-fluoropyridin-3-yloxy)benzamide (1.4 g, 3.81 mmol) and urea peroxide (1.076 g, 11.44 mmol) in 10 mL of DCM at 0 C was added dropwise trifluoroacetic anhydride (1.601 mL, 11.44 mmol) and the resulting reaction was stirred overnight. LCMS showed only less than 50% of desired conversion. The mixture was evaporated to dryness, quenched with Sat. NaHCO3, extracted with EA, dried over Na2SO4, filtered and evaporated to dryness. The crude product was purified using column chromatography (DCM to DCM/EA=3:1 to DCM/MeOH=100:2 to 100:5 to 100:10) to provide 3-(4-bromo-2-(diethylcarbamoyl)phenoxy)-2-fluoropyridine 1-oxide as an offwhite solid.

1. customthe resulting reaction
2. customThe mixture was evaporated to dryness
3. customquenched with Sat. NaHCO3
4. extractionextracted with EA
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customevaporated to dryness
8. customThe crude product was purified