反应详情

A solution of 3-isopropylamino-7-nitro-4H-1,2,4-benzothiadiazine 1,1-dioxide (0.6 g) in hot methanol (25 mL) was supplemented with 10% Pd/C (0.06 g) and submitted to hydrogen under pressure (4 bars) for 1 h at 40° C. The insoluble material was removed by filtration and the filtrate was concentrated to dryness by evaporation under reduced pressure. The residue of the crude title compound was recrystallized from methanol-water (yield: 0.45 g); m.p.: 278-283° C.; IR (KBr): 3455, 3363, 3216, 2972, 1618, 1575, 1510, 1298, 1255, 1174, 1146, 1113 cm−1; 1H-NMR (DMSO-d6, HMDS; d ppm): 1.10 (d, 6H, 2×CH3), 3.85 (m, 1H, NH—CH), 5.15 (bs, 2H, NH2), 6.50-6.95 (bm, 4H, 5-H+6-H+8-H+NH—CH), 9.75 (bs, 1H, NH).

1. customThe insoluble material was removed by filtration
2. concentrationthe filtrate was concentrated to dryness by evaporation under reduced pressure
3. customThe residue of the crude title compound was recrystallized from methanol-water (yield: 0.45 g)