反应详情

To a solution of tert-butyl [(1S,2R)-2-({6-carbamoyl-5-[(4-hydroxy-6-methylpyridin-2-yl)amino]pyridin-3-yl]amino)cyclohexyl}carbamate (32 mg, 0.070 mmol) in DCM (2 ml) was added TFA (1.0 mL, 13 mmol), and the reaction mixture was stirred for 30 minutes at ambient temperature. The reaction mixture was concentrated under reduced pressure, dissolved in DMSO (1 mL), and purified by reverse phase HPLC (acetonitrile/water with 0.1% formic acid, linear gradient) to afford 5-{[(1R,2S)-2-aminocyclohexyl]amino}-3-[(4-hydroxy-6-methylpyridin-2-yl)amino]pyridine-2-carboxamide formic acid salt. MS ESI calc'd. for C18H25N6O2 [M+H]+ 357. found 357. 1H NMR (500 MHz, CD3OD) δ 8.10 (s, 1H), 7.85 (s, 1H), 7.40 (s, 1H), 6.39 (s, 1H), 6.25 (s, 1H), 3.95 (br s, 1H), 3.56 (br s, 1H), 2.38 (s, 3H), 1.90-1.82 (m, 3H), 1.80-1.62 (m, 3H), 1.60-1.50 (m, 2H).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. dissolutiondissolved in DMSO (1 mL)
3. custompurified by reverse phase HPLC (acetonitrile/water with 0.1% formic acid, linear gradient)