反应详情

A solution of 100 mg (0.45 mmol) of 5,6-difluoro-2-methyl-4-oxo-4H-chromene-8-carbaldehyde in 5 ml of 2-propanol is mixed with 46.9 mg (0.45 mmol) of sodium 1-cyanoprop-1-en-2-olate, 63.88 mg (0.45 mmol) of propyl 3-aminocrotonate and 0.04 ml (0.67 mmol) of acetic acid and stirred under reflux for 3 h. After cooling, the mixture is concentrated. The residue is taken up in dichloromethane and washed with water. The organic phase is dried over sodium sulfate and concentrated. The resulting residue is crystallized from diethyl ether. The beige-colored crystals are filtered off with suction and dried at 40° C. in a vacuum drying oven. 74.6 mg (40.35% of theory) of the title compound are obtained.

1. temperatureunder reflux for 3 h
2. temperatureAfter cooling
3. concentrationthe mixture is concentrated
4. washwashed with water
5. dry with materialThe organic phase is dried over sodium sulfate
6. concentrationconcentrated
7. customThe resulting residue is crystallized from diethyl ether
8. filtrationThe beige-colored crystals are filtered off with suction
9. customdried at 40° C. in a vacuum
10. customdrying oven