反应详情

To a solution of compound 145-E (4.94 g, 18.2 mmol) in 5:1 THF/H2O (200 mL) was added LiOH.H2O (0.797 g, 19.0 mmol). The reaction was stirred for 3 days then concentrated in vacuo, to which was added water (100 mL) and 1N HCl (19.0 mL), and the resultant precipitate was isolated by filtration. The solid was rinsed with water and dried under vacuum to afford compound 145-F as a tan-yellow solid (4.51 g, 96%). 1H-NMR (DMSO-d6): δ 7.62 (dd, 1H), 8.62 (dd, 1H), 8.86 (dd, 1H), 14.18 (br s, 1H); MS: m/z 257.9 (MH+).

1. concentrationthen concentrated in vacuo, to which
2. additionwas added water (100 mL) and 1N HCl (19.0 mL)