反应详情

温度

70 °C

A mixture of 2-chloro-N-(5-isopropoxy-1H-pyrazol-3-yl)-5-nitropyrimidin-4-amine (Intermediate 30, 1.0 g) and [(1S)-1-(5-fluoropyridin-2-yl)ethyl]amine hydrochloride (Intermediate 5, 0.8 g) in n-BuOH (5 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 1.0 g of the title compound. MS (electrospray): 403 (M+1) for C17H19FN8O3. 1H NMR (300 MHz, CD3OD) δ ppm 9.10 (s, 1H) 8.50 (s, 1H) 7.60 (m, 1H) 7.40 (m, 1H) 5.80 (s, 1H) 5.20 (m, 1H) 4.70 (m, 2H) 1.60 (d, 3H) 1.40 (d, 6H).

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)