反应详情

1,1-Dimethylethyl 3-{[(3-hydroxy-5-{[(1S)-1-methyl-2-(methyloxy)ethyl]oxy}phenyl) carbonyl]amino}-1H-pyrazole-1-carboxylate (145 mg, 0.5 mmol), 3-[(2,4,5-trifluorophenyl)sulfonyl]dihydrofuran-2(3H)-one (140 mg, 0.5 mmol) and potassium carbonate (138 mg, 2 mmol) in acetonitrile (4 mL) were heated at 130° C. for 1 hour then 160° C. for a further 1 hour in a microwave reactor. Water was added to the reaction mixture and the phases separated. The aqueous phase was extracted with ethyl acetate (3×20 mL), and the combined organics washed with 1M hydrochloric acid, a saturated sodium bicarbonate solution, brine, dried (MgSO4), filtered and evaporated. The residue was chromatographed on alumina, eluting with 0-10% methanol in DCM, to give the desired compound as a white solid (58 mg).

1. customthe phases separated
2. extractionThe aqueous phase was extracted with ethyl acetate (3×20 mL)
3. washthe combined organics washed with 1M hydrochloric acid
4. dry with materiala saturated sodium bicarbonate solution, brine, dried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customThe residue was chromatographed on alumina
8. washeluting with 0-10% methanol in DCM