反应详情

3-chloro-6-(4-(2-(4-methylpiperazin-1-yl)ethoxy)phenyl)-9-(benzenesulfonyl)-9H-pyrido[2,3-b]indole (203 mg, 0.36 mmol) is added to a solution of Na (83 mg, 3.6 mmol, 10 equiv.) in anhydrous MeOH (3.6 ml). The reaction is carried out at 65° C. for 2 hours, the mixture is then hydrolysed with ethanol and H2O and extracted with ethyl acetate (3×20 ml). The organic layers are dried over MgSO4, filtered, and concentrated under reduced pressure. The crude residue (orange solid) is purified over flash chromatography (eluted with THF/MeOH 9:1) to give the product R347 as a white solid (124 mg, 0.30 mmol) in 83% yield. 1H NMR (300 MHz, (CD3)2C0) δ 12.01 (br s, 1H), 8.74 (d, 1H, J=2.3 Hz), 8.49 (d, 1H, J=1.7 Hz), 8.42 (d, 1H, J=2.5 Hz), 7.76 (dd, 1H, J=1.8, 8.5 Hz), 7.66 (d, 2H, J=8.9 Hz), 7.55 (d, 1H, J=8.5 Hz), 7.06 (d, 2H, J=8.9 Hz), 4.13 (t, 2H, J=5.8 Hz), 2.72 (t, 2H, J=5.8 Hz), 2.38 (br s, 8H).

1. extractionhydrolysed with ethanol and H2O and extracted with ethyl acetate (3×20 ml)
2. dry with materialThe organic layers are dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe crude residue (orange solid) is purified over flash chromatography (eluted with THF/MeOH 9:1)