反应详情

To a solution of 13 (862 mg, 4.49 mmol) in methanol (50 mL) was added 5% Pd/C (50 mg) and the reaction mixture was hydrogenated for 1 h at a pressure of 50 lb/inch2. The reaction mixture was filtered through celite and the celite was washed with methanol. The solvent was removed in vacuo and 707 mg (97% yield) of grey powder 14 was obtained. mp: 159°-160° C. 1H NMR (DMSO-d6, ppm): 10.44 (s, 1 H, NH), 7.01-6.99 (d, 1 H, J=8.5 Hz, Ar--H), 6.60 (d, 1 H, J=2.0 Hz, Ar--H), 6.43-6.40 (dd, 1 H, J=2.4, 8.5 Hz, Ar--H), 5.97 (brs, 1 H, Ar--H), 5.07 (brs, 1 H, OH), 4.50 (brs, 2 H, CH2OH), 4.30 (brs, 2 H, NH2), Anal. (C9H10N2O), C, H, N.

1. filtrationThe reaction mixture was filtered through celite
2. washthe celite was washed with methanol
3. customThe solvent was removed in vacuo