反应详情

A mixture of Example 91a (186.0 mg, 0.436 mmol) and HCl (0.20 mL, 6.6 mmol) in ethanol (6 mL) was heated at 95° C. for 3 hours and cooled. Half of the solvent was evaporated; the resulting suspension was filtered and washed with EtOH. The solids were stirred in saturated NaHCO3 for 30 minutes, filtered, washed with water, and oven-dried to give 72.2 mg of the title compound. 1H NMR (300 MHz, DMSO-d6) ppm 6.30 (s, 2H), 6.85 (s, 1H), 6.91 (s, 1H), 7.15 (m, 1H), 8.12 (s, 1H), 8.21-8.36 (m, 2H), 12.15 (s, brd, 1H). MS (ESI+) m/z 244.8 (M+H)+.

1. temperaturecooled
2. customHalf of the solvent was evaporated
3. filtrationthe resulting suspension was filtered
4. washwashed with EtOH
5. filtrationfiltered
6. washwashed with water
7. customoven-dried