反应详情

To an ice-cooled mixture of 2,2-bis(fluoromethyl)-6-trifluoromethyl-2H-1-benzopyran-4-carboxylic acid (0.20 g) and tetrahydrofuran (3 ml), N,N′-carbonyldiimidazole (0.12 g) was added with stirring and the mixture was stirred for 1 hour. Thereafter, 2-cyanoethylamine (0.06 g) was added and the mixture was stirred first under cooling with ice for 1 hour, then at room temperature for 12 hours. To the reaction mixture, an aqueous solution of potassium carbonate was added, followed by extraction with methylene chloride; the organic layer was washed with water and dried; the solvent was distilled off and the resulting residue was recrystallized with a solvent consisting of a mixture of ethyl acetate and hexane, thereby giving the titled compound (0.20 g) having a melting point of 135-136° C.

1. additionwas added
2. stirringthe mixture was stirred for 1 hour
3. stirringthe mixture was stirred first
4. temperatureunder cooling with ice for 1 hour
5. extractionfollowed by extraction with methylene chloride
6. washthe organic layer was washed with water
7. customdried
8. distillationthe solvent was distilled off
9. customthe resulting residue was recrystallized with a solvent
10. additionconsisting of a mixture of ethyl acetate and hexane