反应详情

温度

40 °C

To a solution of 3-[(3-tert-butyl-1-methyl-1H-pyrazol-5-yl)amino]pyridine-2-carbonitrile (100 mg, 0.39 mmol) in MeOH (1 mL) was added an aqueous solution of KOH (3 M, 1 mL), and the mixture was stirred at 40° C. for 48 h. The organic solvent was removed under reduced pressure, and the aqueous layer was acidified to pH 1 to 2 with 1 N aqueous HCl. The mixture was extracted with ethyl acetate (3×). After removal of the solvent under reduced pressure, the crude residue was subjected to preparative HPLC purification with a gradient elution from 20% to 90% acetonitrile in water to give the above product as an oil (6.2 mg, 6%). 1H NMR (400 MHz, CD3OD) δ 1.35 (s, 9H), 3.72 (s, 3H), 6.80 (s, 1H), 7.39-7.42 (m, 2H), 8.08-8.11 (m, 1H). ES-MS m/z 274.1 (MH+), HPLC RT (min) 1.47.

1. customThe organic solvent was removed under reduced pressure
2. extractionThe mixture was extracted with ethyl acetate (3×)
3. customAfter removal of the solvent under reduced pressure
4. customthe crude residue was subjected to preparative HPLC purification with a gradient elution from 20% to 90% acetonitrile in water