反应详情

(R)-2-(3-Amino-6-(5-methyl-1H-pyrazol-3-ylamino)pyridin-2-ylamino)-2-(4-fluorophenyl)ethanol (Method 62, 0.28 g, 0.82 mmol) and formamidine acetate (0.17 g, 1.6 mmol) in EtOH (5 ml) was heated at reflux overnight. Saturated sodium bicarbonate solution (10 ml) and EtOAc (30 ml) was added. The organic layer was separated, washed with brine (10 ml) and dried over sodium sulfate. The solvent was removed under reduced pressure and the residue was purified by chromatography (EtOAc-MeOH=40:1) to give the title compound as off white solid (0.021 g, 73%). 1H NMR (400 MHz) δ 11.72 (s, 1H), 9.24 (s, 1H), 8.33 (s, 1H), 7.77 (d, J=8.4 Hz, 1H), 7.40 (m, 2H), 7.17 (m, 2H), 6.93 (d, J=8.0 Hz, 1H), 6.27 (s, 1H), 5.71 (br s, 1H), 5.32 (t, J=4.2 Hz, 1H), 4.34 (m, 1H), 4.12 (m, 1H), 4.03 (m, 1H), 2.22 (s, 3H). MS: Calcd.: 352. Found: [M+H]+ 353.

1. temperatureat reflux overnight
2. customThe organic layer was separated
3. washwashed with brine (10 ml)
4. dry with materialdried over sodium sulfate
5. customThe solvent was removed under reduced pressure
6. customthe residue was purified by chromatography (EtOAc-MeOH=40:1)