反应详情

A solution of KOH (1.68 g, 30 mmol) in water (25 mL) and MeOH (25 mL) was added to Intermediate 1 (5.8 g, 30 mmol), and the resulting mixture was stirred for 18 hours at room temperature. The reaction was diluted with water, then extracted with EtOAc. The aqueous layer was cooled in an ice bath, acidified with 1N HCl, extracted with EtOAc, dried (Na2SO4), and concentrated in vacuo to provide 3.8 g (77%) of a colorless solid. 1H NMR (DMSO-d6) δ: 7.1–7.8 (m, 6H), 10.5 (s, 1H); MS ES+m/e 166.0 (p+1), ES−m/e 164.1 (p−1). Anal. Calcd for C8H7NO3: C, 58.18; H, 4.27; N, 8.48. Found: C, 57.99; H, 4.25; N, 8.46.

1. extractionextracted with EtOAc
2. temperatureThe aqueous layer was cooled in an ice bath
3. extractionextracted with EtOAc
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated in vacuo