反应详情

A solution of Intermediate 12B (18.6 g, 47 mmol) in AcOH (200 mL), H2O (150 mL) and H2SO4 (2.0 mL) was stirred at 110° C. for 4 h. Most of the solvent was removed and the residue was diluted with EtOAc (400 mL), washed with H2O (5×20 mL), saturated NaHCO3, 1N NaOH, and brine. The solvent was removed to give Intermediate 12C (10 g, 84% yield) as a low melting solid. 1H NMR (400 MHz, DMSO-d6) δ 7.42 (q, J=6.8, 6.4 Hz, 1H), 7.24 (q, J=6.4, 5.2 Hz, 1H), 2.5 (s, 3H) ppm.

1. customMost of the solvent was removed
2. additionthe residue was diluted with EtOAc (400 mL)
3. washwashed with H2O (5×20 mL), saturated NaHCO3, 1N NaOH, and brine
4. customThe solvent was removed