反应详情

6-Methyl-5-(6-(trifluoromethyl)-1H-indazol-4-yl)picolinonitrile (0.02 g, 0.066 mmol) in acetic acid (2 mL) and H2SO4 (2 mL) was stirred at room temperature for 18 hours. The reaction mixture was subsequently poured into a conical flask containing ice and was carefully neutralized with NaHCO3 and extracted into DCM. The organic layer was dried over Na2SO4 and concentrated in vacuo. The residue was purified by preparative HPLC (Waters SunFire C18, 5 μm, 30 mm ID×75 mm column) eluting with a gradient of 45-55% ACN (containing 0.035% TFA) in water (containing 0.05% TFA) to give the title compound as white solid (0.32 g, 34%). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.42 (s, 3H), 7.42 (d, J=1.26 Hz, 1H), 7.73 (br s, 1H), 7.90-8.08 (m, 3H), 8.14 (br s, 1H); ESI-MS m/z [M+H]+ calc'd for C15H11F3N4O, 321.1. found 321.2.

1. additionThe reaction mixture was subsequently poured into a conical flask
2. additioncontaining ice
3. extractionextracted into DCM
4. dry with materialThe organic layer was dried over Na2SO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by preparative HPLC (Waters SunFire C18, 5 μm, 30 mm ID×75 mm column)
7. washeluting with a gradient of 45-55% ACN (containing 0.035% TFA) in water (containing 0.05% TFA)