反应详情

温度

0 °C

To a cooled (0° C.), stirred solution of 2-{3,5-dichloro-4-[4-methoxy-3-(piperidine-1-sulfonyl)-phenoxy]-phenyl}-2H-[1,2,4]triazine-3,5-dione (0.5 g) in dichloromethane (30 mL) was added boron tribromide (0.3 mL) and the resulting heterogeneous mixture was allowed to stir at room temperature for 6 h. Ice was added to the mixture and the resulting two-phase solution stirred for 1 h. Layers were separated and the organic phase was washed with water, brine, dried (Na2SO4) and concentrated in vacuo to afford an oil. Flash chromatography on silica gel (35% acetone/hexanes) afforded the title compound of this EXAMPLE as a colorless solid, 0.4 g. MS Calc.:513.4 Found:512.9.

1. additionIce was added to the mixture
2. stirringthe resulting two-phase solution stirred for 1 h
3. customLayers were separated
4. washthe organic phase was washed with water, brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated in vacuo
7. customto afford an oil