反应详情

To a solution of Example 4 (84 mg, 0.22 mmol) in DMF (1.1 mL), 10% Pd on charcoal (10 mg) and ammonium formate (68 mg, 1.08 mmol) were added. The mixture was stirred at RT for 20 h then filtered through Celite® and concentrated in vacuo. The resulting solid was dissolved in methanol and purified by SCX-silica column (18 g) by washing with methanol (2×8 mL) and then by eluting a solution of 2M ammonia in methanol (2×8 mL) to give the title compound (60 mg, 93%) as a beige solid. 1H NMR (400 MHz, DMSO-d6) δ 12.16 (1H, s), 9.53 (1H, s), 8.29 (1H, d, J=9.6 Hz), 7.88 (1H, s), 7.61 (1H, t, J=3.0 Hz), 7.55 (1H, s), 6.59 (1H, dd, J=2.0, 3.5 Hz), 2.40 (3H, s). LC/MS=m/z 300 (M+H)+.

1. filtrationthen filtered through Celite®
2. concentrationconcentrated in vacuo
3. dissolutionThe resulting solid was dissolved in methanol
4. custompurified by SCX-silica column (18 g)
5. washby washing with methanol (2×8 mL)
6. washby eluting a solution of 2M ammonia in methanol (2×8 mL)