反应详情

温度

2.5 °C

A solution of 2-amino-N-(4-methoxy-quinolin-8-yl)-4-trifluoromethyl-benzenesulfonamide (Intermediate 196) (454 mg, 1.1 mmol) in AcOH/THF (1:1, 10 ml) was cooled to 0° C. and tert-butylnitrite (235 mg, 2.2 mmol) was added. The reaction was stirred at 0-5° C. for 2 h. The reaction was quenched water (5 ml) and the solvent partially evaporated. The residue was dissolved in EtOAc (150 ml), washed with sat. sodium bicarbonate solution, dried (MgSO4) and concentrated in vacuo. The crude residue was purified by column chromatography with DCM/MeOH (1:0-99:1) gradient elution followed by recrystallisation from iPA/MeCN to give the title compound (45 mg, 11%).

1. customThe reaction was quenched water (5 ml)
2. customthe solvent partially evaporated
3. dissolutionThe residue was dissolved in EtOAc (150 ml)
4. washwashed with sat. sodium bicarbonate solution
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. customThe crude residue was purified by column chromatography with DCM/MeOH (1:0-99:1) gradient elution
8. customfollowed by recrystallisation from iPA/MeCN