反应详情

Reflux bisazaindole 35 (40 mg, 0.066 mmol) in KOH at 3%/MeOH (10 mL) for 16 h, then concentrate under vacuum. The residue is dissolved in EtOAc, washed with saturated NaHCO3, dried (Na2SO4) and submitted to flash chromatography on SiO2 (MeOH at 4%/CH2Cl2, 0.25% of NH3) to give 36 (18 mg, 60.2%) as a white solid: 1H NMR (CDCl3. δ 10.94 (s broad, 1H), 8.07 (d, 1H, J=5.2 Hz), 7.61 (s, 1H), 7.15 (s, 1H), 7.05 (d, 1H, J=5.2 Hz), 6.65 (d, 1H, J=2 Hz), 4.23 (s overlapping t, 5H, J=6.5 Hz), 3.97 (s, 3H), 2.79 (t, 2H, J=6.5 Hz), 2.55-2.45 (m broad, 8H), 2.29 (s, 3H), TLC (MeOH at 10%/CH2Cl2, 0.25% of NH3) Rf=0.35, m/z obs.=455.11 (M+1).

1. concentrationconcentrate under vacuum
2. dissolutionThe residue is dissolved in EtOAc
3. washwashed with saturated NaHCO3
4. dry with materialdried (Na2SO4)