反应详情

温度

0 °C

2-Amino-N-quinolin-8-yl-4-trifluoromethyl-benzenesulfonamide (Example Compound 35) (50 mg, 0.14 mmol) was dissolved in acetic acid/THF (1:1; 2 ml) and cooled to 0° C. Tert-butylnitrite (16.2 μl, 0.14 mmol) was added and the mixture was stirred for 1 h keeping the temperature between 0° C. -5° C. The reaction was quenched with water (3 ml), while keeping the temperature between 0° C. -5° C., and the organic phase was extracted with EtOAc (10 ml). The combined organic phases were washed with sat. sodium bicarbonate and concentrated in vacuo. The crude residue was purified by column chromatography with DCM as the eluent to give the title compound (11 mg, 23%)

1. custombetween 0° C. -5° C
2. customThe reaction was quenched with water (3 ml)
3. custombetween 0° C. -5° C.
4. extractionthe organic phase was extracted with EtOAc (10 ml)
5. washThe combined organic phases were washed with sat. sodium bicarbonate
6. concentrationconcentrated in vacuo
7. customThe crude residue was purified by column chromatography with DCM as the eluent