HCID 59458015, compound → HCID 59458012, compound

Participants

Reaction Steps

To a suspension of 11 (790 mg, 2.16 mmol) in 1:1 MeOH/THF (100 ml) was added 10% Pd/C (100 mg) and hydrogenated at 45 Hg mm. for 20 h. The reaction mixture was filtered and evaporated to dryness and recrystallized from DCM/Pert.ether to give 12 (695 mg, 96%); mp (DCM/pet.ether)>300° C.; 1H NMR [(CD3)2SO] δ 9.78 (s, 1 H, NH), 9.45 (s, 1 H, NH), 8.63 (dd, J=2.4, 0.3 Hz, 1 H, H-2′), 8.09 (d, J=9.0 Hz, 1 H, H-5′), 7.98 (dd, J=9.0, 2.6 Hz, 1 H, H-4′), 7.72 (d, J=8.7 Hz, 2 H, H-2,6), 6.61 (d, J=8.7 Hz, 2 H, H-3,5), 6.43 (s, 1 H, H-5″), 6.13 (s, 2 H, NH2), 5.73 (s, 2 H, NH2), 2.12 (s, 3 H, CH3); HRMS (FAB+) calc. for C17H18N7O (M+1) m/z 336.1573, found 336.1578; Anal. calc. for C17H17N7O-0.25H2O: C, 60.1; H, 5.2; N, 28.9; C, 60.2; N, 5.3; N, 29.0%.

Provenance & Evidence