反应详情

To a stirred solution of 38 (2.5 g, 7.18 mmol) in THF (50 ml) was added KOH (14.3 ml, 1.0 N in H2O, 14.3 mmol). After 4 hours the reaction mixture was concentrated and the resultant residue was dissolved in H2O (50 ml). The aqueous layer was then washed with ethyl acetate and acidified with 1N HCl (pH=1). The precipitate that formed upon acidification was collected by filtration, washed with water and dried under high vacuum to afford title compound 39 (2.3 g, 96% yield) as a white solid 1H NMR (400 MHz, DMSO-d6) δ(ppm): 8.68 (d, J=5.2 Hz, 1H), 8.47 (dd, J=2.8 and 10.4 Hz, 1H), 8.20 (m, 1H), 8.17 (s, 1H), 7.76 (dd, J=8.0 and 8.8 Hz, 1H), 7.04 (d, J=5.2 Hz, 1H).

1. concentrationAfter 4 hours the reaction mixture was concentrated
2. dissolutionthe resultant residue was dissolved in H2O (50 ml)
3. washThe aqueous layer was then washed with ethyl acetate
4. customThe precipitate that formed upon acidification
5. filtrationwas collected by filtration
6. washwashed with water
7. customdried under high vacuum