HCID 67199810, compound → HCID 86621654, compound

Participants

Reaction Steps

To a suspension of 16 (6.0 g, 20 mmol) was added 2N HCl (40 mL) and the mixture was refluxed for 20 h. The solvents were evaporated to dryness, residue boiled in MeOH and diluted with EtOAc. The resulting precipitate was filtered and washed with EtOAc and dried to give essentially pure 17 (5.0 g, 97%); mp (MeOH/EtOAc) 275-280° C.; 1H NMR [(CD3)2SO] δ 12.50 (br, 1 H, N+H), 10.75 (br s, 1 H, NH), 9.75 (br s, 2 H, NH2), 7.85 (br s, 4 H, NH2 & ArH)), 7.34 (d, J=8.6 Hz, 2 H, ArH), 6.24 (br s, 1 H, ArH), 2.79 (s, 3 H, CH3), HRMS (FAB+) calc. for C11H14N5 (M+1) m/z 216.1249, found 216.1247.

Provenance & Evidence