Sulfamide → Phenyl-1,3-dihydro-2-thia-1,3,9-triaza-cyclopenta[a]naphthalene 2,2-dioxide
反応式
[S:1](N)(N)(=[O:3])=[O:2].[C:6]1([NH:12][C:13]2[C:22]([NH2:23])=[C:21]3[C:16](C=CC=N3)=[CH:15][CH:14]=2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>N1C=CC=CC=1>[C:6]1([N:12]2[C:13]3=[C:14]4[C:15](=[CH:16][CH:21]=[C:22]3[NH:23][S:1]2(=[O:3])=[O:2])[CH:8]=[CH:7][CH:6]=[N:12]4)[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1参加物
4
反応条件
- 温度
- 115 °C
実験手順
Sulfamide (34 mg, 0.35 mmol) was added to a solution of N*7*-phenyl-quinoline-7,8-diamine 576 (56 mg, 0.23 mmol) in pyridine (2 ml) and the mixture was heated in a microwave at 115° C. for 2 h. After cooling, the solvent was removed in vacuo. The residue was dissolved in EtOAc (50 ml) and the organic phase was washed with sat. NaHCO3 solution (30 ml), dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by column chromatography DCM/MeOH/TEA (98:2:0.5-90:10:0.5 gradient) followed by preparative HPLC (acidic conditions 1) to give the title compound (12.3 mg, 17%).