反应详情

温度

50 °C

2 g (8.5 mmol) of 3-phenyl-1,7-naphthyridine-5-carboxaldehyde are suspended in 20 ml of ethanol and stirred with 0.7 ml (8.5 mmol) of 5-methylisoxazole. A solution of 196 mg of sodium in 14 ml of ethanol is added and the mixture is stirred for 2 hours at 50° C. 1.42 g of ethyl amidinoacetate hydrochloride and 0.51 ml (8.5 mmol) of acetic acid are added and the mixture is boiled for 16 hours. After cooling, 10 g of silica gel are added and the mixture is concentrated in vacuo. The residue is chromatographed on a silica gel column using toluene/ethyl acetate mixtures. After concentration of the pure fractions, the product is crystallized by trituration with ether. 2 g of crystals are obtained.

1. waitthe mixture is boiled for 16 hours
2. temperatureAfter cooling
3. addition10 g of silica gel are added
4. concentrationthe mixture is concentrated in vacuo
5. customThe residue is chromatographed on a silica gel column
6. customAfter concentration of the pure fractions, the product is crystallized by trituration with ether