反应详情

To 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-(1,3-dithiolan-2-yl)-1H-pyrazole-3-carbonitrile (0.30 g, 0.71 mmol) in triethyl orthoformate (4.45 g, 29.70 mmol) was added p-toluenesulfonic acid (18 mg). The resulting mixture was heated up to 100 C for 1.5 hr. It was then cooled and then concentrated. The resulting viscous liquid was diluted with dichloromethane (20 mL). The organic layer was washed with saturated sodium bicarbonate, brine, and then dried over sodium sulfate to provide, upon concentration, a yellow oil (0.35 g, 0.72 mmol); 19F-NMR: −63.698.

1. temperatureThe resulting mixture was heated up to 100 C for 1.5 hr
2. temperatureIt was then cooled
3. concentrationconcentrated
4. additionThe resulting viscous liquid was diluted with dichloromethane (20 mL)
5. washThe organic layer was washed with saturated sodium bicarbonate, brine
6. dry with materialdried over sodium sulfate
7. customto provide, upon concentration