反应详情

温度

70 °C

A mixture of 2-chloro-N-(5-cyclopropyl-1H-pyrazol-3-yl)-5-nitropyrimidin-4-amine (Intermediate 17, 0.35 g) and [(1S)-1-(5-fluoropyrimidin-2-yl)ethyl]amine hydrochloride (Intermediate 15, 0.25 g) in n-BuOH (10 mL) with diisopropylethylamine (1 mL) was stirred at 70° C. for 4 hours. The resulting mixture was diluted with ethyl acetate (20 mL), and washed with brine (10 mL×3). The organic layer was dried and concentrated. The resulting residue was separated by silica gel column (Hexane/Ethyl acetate) to yield 0.3 g of desired product. MS (electrospray): 386 (M+1) for C16H16FN9O2. 1H NMR (300 MHz, DMSO-d6) δ ppm 12.4 (s, 1H) 11.30 (s, 1H) 9.15 (s, 1H) 9.00 (s, 1H) 8.80 (s, 2H) 6.10 (d, 1H) 5.25 (m, 1H), 1.90 (m, 1H) 1.60 (d, 3H) 1.00 (m, 2H) 0.80 (m, 2H).

1. washwashed with brine (10 mL×3)
2. customThe organic layer was dried
3. concentrationconcentrated
4. customThe resulting residue was separated by silica gel column (Hexane/Ethyl acetate)