反应详情

A solution of 310 mg (1.03 mmol) of ethyl 2-[(2-methyl-4-oxo-4H-chromen-8-yl)methylene]-3-oxobutanoate in 30 ml of 2-propanol is mixed with 140.47 mg (1.03 mmol) of 3-amino-4,4,4-trifluorobut-2-enenitrile [preparation analogous to K. Krespan, J. Org. Chem. 34, 42-45 (1969)] and 17.38 mg (0.15 mmol) of potassium tert-butoxide and stirred under reflux for 12 h. After cooling, the mixture is concentrated. The residue is purified on an Analogix cartridge (F12M) (mobile phase: cyclohexane/ethyl acetate 2:1). After concentration of the product fractions, the residue is crystallized from diethyl ether. 50.9 mg (10.8% of theory) of the title compound are obtained as white crystals.

1. temperatureunder reflux for 12 h
2. temperatureAfter cooling
3. concentrationthe mixture is concentrated
4. customThe residue is purified on an Analogix cartridge (F12M) (mobile phase: cyclohexane/ethyl acetate 2:1)
5. customAfter concentration of the product fractions, the residue is crystallized from diethyl ether