反应详情

温度

0 °C

To a cooled (0° C.), stirred solution of N-{5-[2,6-dichloro-4-(3,5-dioxo-4,5-dihydro-3H-[1,2,4]triazin-2-yl)-phenoxy]-2-methoxy-phenyl}-4-fluoro-benzenesulfonamide (96 mg) in dichloromethane (5 mL) was added boron tribromide (64 μL) and the resulting solution was allowed to stir at ambient temperature for 4 h. The reaction mixture was poured over ice, stirred for 0.5 h and extracted with ethyl acetate. The organic phase was dried (Na2SO4), concentrated in vacuo and flash chromatographed on silica gel (40% acetone/hexanes) to afford the title compound of this EXAMPLE as a colorless foam, 68 mg. m.p. 222-225° C. (dec), MS Calc.:539.2 Found:536.8.

1. additionThe reaction mixture was poured over ice
2. stirringstirred for 0.5 h
3. extractionextracted with ethyl acetate
4. dry with materialThe organic phase was dried (Na2SO4)
5. concentrationconcentrated in vacuo and flash
6. customchromatographed on silica gel (40% acetone/hexanes)