反应详情

温度

2.5 °C

Furan-2-carboxylic acid (0.8 g; 7 mmol) in 15 ml of dichloromethane was cooled to 0° C., and 0.76 g of 1,3-dicyclohexylcarbodimide (4 mmol) was added slowly. The reaction mixture was stirred at 0-5° C. for 2 hours and filtered. The filtrate was evaporated, the residue was dissolved in 15 ml of pyridine and added 0.43 g of N-hydroxy-nicotinamidine (3.2 mmol). The reaction mixture was heated at reflux until the reaction was finished (measured by TLC), then cooled to room temperature and poured into 100 ml of water. The precipitate was isolated by filtration and dried under vacuum. The product was isolated by column chromatography. Yield 0.23 g (15%). Mp. 110-114° C.

1. filtrationfiltered
2. customThe filtrate was evaporated
3. dissolutionthe residue was dissolved in 15 ml of pyridine
4. temperatureThe reaction mixture was heated
5. temperatureat reflux until the reaction
6. temperaturecooled to room temperature
7. customThe precipitate was isolated by filtration
8. customdried under vacuum
9. customThe product was isolated by column chromatography