反应详情

温度

80 °C

To N-(5-chloro-2-{3-[4-(4-hydroxypiperidine-1-sulfonyl)-phenyl]-propionyl}-phenyl)-2-oxo-N-phenyl-propionamide in MeOH was added K2CO3 (0.096 g), and the mixture heated at 80° C. for 1.5 h, then concentrated. The residue was taken up in EtOAc/H2O, and the aqueous layer washed with EtOAc (2×25 mL). The combined organic layers were dried over Na2SO4, and the solvent removed under reduced pressure. The residue was chromatographed on anhydrous silica (20% EtOAc/hexanes 0-5 min; 60% EtOAc/hexanes 15-20 min; 100% EtOAc 22-35 min) to provide 2-acetyl-7-chloro-3-[4-(4-hydroxypiperidine-1-sulfonyl)-benzyl]-1-phenyl-1H-quinolin-4-one (compound 70). Mp=145.5-147.2° C.; M+H 551.

1. concentrationconcentrated
2. washthe aqueous layer washed with EtOAc (2×25 mL)
3. dry with materialThe combined organic layers were dried over Na2SO4
4. customthe solvent removed under reduced pressure
5. customThe residue was chromatographed on anhydrous silica (20% EtOAc/hexanes 0-5 min; 60% EtOAc/hexanes 15-20 min; 100% EtOAc 22-35 min)