HCID 67199568, compound → HCID 67202012, compound

Participants

Reaction Steps

To a suspension of (A3 (1.75 g, 4.88 mmol) in MeOH (10 mL) was added 10% Pd/C (0.1 g) and hydrogenated (under 40 psi). for 2 h. The reaction mixture was filtered and washed with more MeOH. The filtrated was concentrated to half the volume, diluted with EtOAc and the rest of the MeOH was evaporated. The Resulting precipitate was filtered washed with more EtOAc and dried to give essentially pure (A4) (1.255 g 78%); mp (MeOH/EtOAc)>280° C.; 1H NMR [(CD3)2SO] δ13.95 (br, 1 H, N+H), 10.14 (s, 1 H, NH), 10.01 (s, 1H, NH), 8.10 (d, J=6.7 Hz, 1 H, ArH), 7.74 (d, J=8.9 Hz, 3 H, ArH), 7.43 (d, J=2.2 Hz, 1 H, ArH), 7.38-7.32 (m, 3 H, ArH), 6.61 (d, J=6.7 Hz, 1 H, ArH), 5.94 (s, 2 H, NH2), 2.08 (s, 3 H, COCH3); APCI+ve 293.

Provenance & Evidence