反应详情

A suspension of 146 (200 mg, 0.36 mmol) in anhydrous MeOH (10 mL) was hydrogenated in the presence of 10% Pd/C (100 mg) at 25° C. for 20 min. The catalyst and precipitate were collected and dissolved in 10% NaHCO3 solution and then filtered. The filtrate was acidified with dil aq HCl and the precipitate was then collected and washed with acetone to give 147 (97 mg, 0.25 mmol). Yellow solid; yield: 69.8%; mp>300° C.; MS (ESI): m/z 387.1 (M+H)+; 1H-NMR (D2O+NaOD, 200 MHz): δ 1.78 (m, 4H), 3.08 (m, 4H), 6.70 (s, 1H), 7.12-7.20 (m, 3H), 7.28 (t, J=7.8 Hz, 1H), 7.40 (d, J=7.6 Hz, 1H), 7.49 (s, 1H), 7.61 (d, J=9.8 Hz, 1H); Anal. (C19H19N2O5P) C, H, N.

1. customThe catalyst and precipitate were collected
2. dissolutiondissolved in 10% NaHCO3 solution
3. filtrationfiltered
4. customthe precipitate was then collected
5. washwashed with acetone