反应详情

A mixture of (R)-2-[5-amino-4-(5-cyclopropyl-1H-pyrazol-3-ylamino)-6-methylpyrimidin-2-ylamino]-2-(4-fluorophenyl)ethanol (Method 40; 0.3 g, 0.8 mmol) and formamidine acetate (0.2 g, 1.6 mmol) in EtOH (8 ml) was heated to reflux for 12 hours. The reaction was then concentrated, dissolved in DCM (50 ml), and washed with saturated NaHCO3 solution (50 ml). The organic layer was then dried, filtered, and concentrated. The resulting solid was purified by column chromatography (DCM:MeOH=20:1) to give the title compound (0.11 g, 35%). NMR (400 MHz, CD3OD) 8.32 (s, 1H), 7.46-7.43 (m, 2H), 7.06-7.02 (m, 2H), 6.24 (s, 1H), 5.10-5.02 (m, 1H), 3.87-3.75 (m, 2H), 2.61 (s, 3H), 1.99-1.96 (m, 1H), 1.10-1.08 (m, 2H), 0.80-0.75 (m, 2H). MS: Calcd.: 393; Found: [M+H]+ 394.

1. temperaturewas heated
2. temperatureto reflux for 12 hours
3. concentrationThe reaction was then concentrated
4. dissolutiondissolved in DCM (50 ml)
5. washwashed with saturated NaHCO3 solution (50 ml)
6. customThe organic layer was then dried
7. filtrationfiltered
8. concentrationconcentrated
9. customThe resulting solid was purified by column chromatography (DCM:MeOH=20:1)