反应详情

A solution of compound 4 (0.8 g, 1.815 mmol) in methanol (10 mL) was treated with 1 N HCl (10 mL) and the resulting mixture was refluxed for 30 minutes. The reaction was brought to room temperature and solvent was evaporated. The crude product was dissolved into water (10 mL), filtered and washed. Water was evaporated to obtain compound 48 (0.7 g, 93%) as a solid. 1H NMR (DMSO-d6) δ 11.44 (s, 1H), 9.78-9.65 (m, 3H), 8.78 (s, 1H), 8.17-8.15 (m, 2H), 7.37 (t, 1H, J=4.2 Hz), 7.20-7.08 (m, 3H), 3.50-3.40 (m, 1H), 3.38-3.26 (m, 1H), 3.17-2.90 (m, 4H), 2.76 (brt, 2H), 2.30-2.20 (m, 1H), 2.00-1.90 (m, 1H), 1.70-1.50 (m, 4H); ESI-MS (m/z, %): 341 (MH+, 38), 272 (100); ESI-HRMS calculated for C19H25N4S (MH+, free base), calculated: 341.1794; observed: 341.1801; HPLC-purity: 98.20% by area.

1. temperaturethe resulting mixture was refluxed for 30 minutes
2. customwas brought to room temperature
3. customsolvent was evaporated
4. dissolutionThe crude product was dissolved into water (10 mL)
5. filtrationfiltered
6. washwashed
7. customWater was evaporated