反应详情

While stirring at room temperature, 1.8 ml of triethylamine and 2.8 ml of DPPA were added in that order to 100 ml of t-butanol solution containing 1.5 g of 2-cyanoisonicotinic acid, and the mixture was heated under refulx for 4 hours and 25 minutes. The reaction mixture was cooled to room temperature, mixed with water and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium bicarbonate and dried over anhydrous sodium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by a silica gel column chromatography, and 1.34 g of the title compound was obtained from ethyl acetate-hexane (1:2, v/v) eluate.

1. temperaturethe mixture was heated under refulx for 4 hours and 25 minutes
2. temperatureThe reaction mixture was cooled to room temperature
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with saturated aqueous sodium bicarbonate
5. dry with materialdried over anhydrous sodium sulfate
6. customthe solvent was evaporated under reduced pressure
7. customThe residue was purified by a silica gel column chromatography