反应详情

温度

100 °C

A mixture of 4-bromo-2,2-bis(fluoromethyl)-6-trifluoromethyl-2H-1-benzopyran (1.73 g), 2-cyanoethylamine (1.44 g), potassium iodide (0.86 g), triphenylphosphine (26 mg), palladium acetate (11 mg) and N,N-dimethylacetamide (10 ml) was stirred under a CO atmosphere at 100° C. for 3 hours. To the reaction mixture, 2 N HCl was added and the precipitating crystals were recovered by filtration. To the recovered crystals, ethyl acetate was added and the insoluble matter was filtered off; the filtrate was washed with a saturated aqueous solution of sodium thiosulfate and a saturated aqueous solution of sodium chloride, dried with anhydrous sodium sulfate and concentrated under reduced pressure; the resulting residue was recrystallized with an ethanol/water mixed solvent, thereby giving N-(2-cyanoethyl)-2,2-bis(fluoromethyl)-6-trifluoromethyl-2H-1-benzopyran-4-carboxamide (1.46 g) having a melting point of 129-131° C.

1. filtrationthe precipitating crystals were recovered by filtration
2. additionTo the recovered crystals, ethyl acetate was added
3. filtrationthe insoluble matter was filtered off
4. washthe filtrate was washed with a saturated aqueous solution of sodium thiosulfate
5. dry with materiala saturated aqueous solution of sodium chloride, dried with anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customthe resulting residue was recrystallized with an ethanol/water mixed solvent