反应详情

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.

1. temperaturethe mixture was refluxed for 20 h
2. customThe solvents were evaporated to dryness, residue
3. additiondiluted with EtOAc
4. filtrationThe resulting precipitate was filtered
5. washwashed with EtOAc
6. customdried