反应详情

温度

40 °C

Under a nitrogen atmosphere, 4-fluoro-N-hydroxybenzenecarboximidoyl chloride (7.6 g, 44 mmol) was added to a heated solution (40° C.) of 3-nitro-N-prop-2-ynyl[1,5]naphthyridin-4-amine (5.0 g, 22 mmol) and anhydrous triethylamine (6.7 mL, 48 mmol) in anhydrous dichloromethane (150 mL). The reaction was heated at 40° C. for 1.7 hours and then concentrated under reduced pressure. The residue was triturated with water; the resulting solid was isolated by filtration, washed sequentially with toluene and a small amount of diethyl ether, and then dissolved in dichloromethane. The solution was concentrated under reduced pressure and dried under high vacuum to provide 6.00 g of N-{[3-(4-fluorophenyl)isoxazol-5-yl]methyl}-3-nitro[1,5]naphthyridin-4-amine as a brownish-yellow solid.

1. concentrationconcentrated under reduced pressure
2. customThe residue was triturated with water
3. customthe resulting solid was isolated by filtration
4. washwashed sequentially with toluene
5. dissolutiona small amount of diethyl ether, and then dissolved in dichloromethane
6. concentrationThe solution was concentrated under reduced pressure
7. customdried under high vacuum