反应详情

A mixture of 26.1 g. (0.15 mole) of 4-oxo-4H-1-benzopyran-3-carboxaldehyde, 13.1 g. (0.19 mole) of hydroxylamine hydrochloride, 18.4 g. (0.27 mole) of sodium formate and 250 ml of 99% formic acid was heated with stirring at reflux for 21/2 hours. Water was added to 1-liter volume. The separated solid was filtered from the cooled mixture, washed well with water and dried to give 13 g. (51%) of crude nitrile melting at 138°-145°C. Recrystallization from ethylacetate gave pure, white crystals melting at 174°-176°.

1. additionA mixture of 26.1 g
2. temperatureat reflux for 21/2 hours
3. filtrationThe separated solid was filtered from the cooled mixture
4. washwashed well with water
5. customdried
6. customto give 13 g
7. customRecrystallization from ethylacetate
8. customgave pure