反应详情

To a stirred solution of 3-bromo-6-difluoromethoxy-2-(3-fluoro-phenyl)-pyrazolo[1,5-b]pyridazine (286 mg) in DMF(20 ml) was added 2N aq sodium carbonate (10 ml). To this mixture was added 4-methanesulfonyl-phenylboronic acid (180 mg) and tetrakis triphenylphosphine palladium (0) (34 mg). The resulting mixture was stirred and heated to reflux for 18 hours. The cooled reaction mixture was diluted with ethyl acetate (300 ml) and the organic solution washed with water (10×30 ml) and brine (30 ml), dried (Na2SO4) and evaporated to give a gum which was purified by flash column chromatography with chloroform:ethyl acetate (50:1to 5:1) as eluant. Combination of appropriate fractions and concentration gave the title compound as an off-white solid (132 mg, 37%).

1. temperatureheated
2. temperatureto reflux for 18 hours
3. customThe cooled reaction mixture
4. washthe organic solution washed with water (10×30 ml) and brine (30 ml)
5. dry with materialdried (Na2SO4)
6. customevaporated
7. customto give a gum which
8. customwas purified by flash column chromatography with chloroform:ethyl acetate (50:1to 5:1) as eluant
9. concentrationCombination of appropriate fractions and concentration