反应详情

A solution of 230 mg (0.72 mmol) of ethyl 2-[(6-fluoro-2-methyl-4-oxo-4H-chromen-8-yl)-methylene]-3-oxobutanoate in 10 ml of 2-propanol is mixed with 98.34 mg (0.72 mmol) of 3-amino-4,4,4-trifluorobut-2-enenitrile [preparation in analogy to K. Krespan, J. Org. Chem. 34, 42-45 (1969)] and 12.2 mg (0.11 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). The resulting crystals are purified further by preparative HPLC. 27.4 mg (8.69% of theory) of the title compound are obtained as yellow 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. customThe resulting crystals are purified further by preparative HPLC