反应详情

Lithium hydroxide (1N, 100 mL) was added to a solution of Example 1A (19.6 g, 46.6 mmol) in THF (50 mL), and the reaction was stirred for 16 h. The solution was acidified to pH=3 with 1N HCl. The resulting solid was collected by filtration and dried under vacuum to give 12.6 g (69%) of the title compound. H1-NMR (DMSO-d6): δ 8.90 (s, 1H), 8.58 (t, 1H, J=4.8 Hz), 8.01 (d, 1H, J=2.0 Hz), 7.73 (d, 1H, J=3.6 Hz), 7.66 (d, 1H, J=3.6 Hz), 7.58 (t, 1H, J=3.6 Hz), 7.52 (t, 1H, J=3.6 Hz), 5.10 (d, 2H, J=4.8 Hz), 4.02 (s, 3H), 3.91 (s, 3H). MS (ES) (M+H) calc'd for C21H16N2O6, 393; found 393.

1. filtrationThe resulting solid was collected by filtration
2. customdried under vacuum