反应详情

温度

115 °C

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%).

1. temperatureAfter cooling
2. customthe solvent was removed in vacuo
3. dissolutionThe residue was dissolved in EtOAc (50 ml)
4. washthe organic phase was washed with sat. NaHCO3 solution (30 ml)
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated in vacuo
7. customThe crude residue was purified by column chromatography DCM/MeOH/TEA (98:2:0.5-90:10:0.5 gradient)