反应详情

温度

50 °C

Into a 500 ml SUS autoclave, 45.4 g (purity: 98%, 0.272 mol) of 2-chloro-3,5-difluoroaniline, 1.84 g of 5% palladium-carbon, 30.2 g (0.299 mol) of triethylamine and 45.4 g of water were introduced, and hydrogen gas was sealed in. Then, the mixture was reacted under a hydrogen gas pressure of 15 kg/cm2 at a temperature of 100° C. for 4 hours. Then, the reaction solution was cooled to 50° C. Then, palladium-carbon was filtered off, and 50 g of a 25% sodium hydroxide aqueous solution was added. The mixture was stirred and left to stand still. Then, the oil layer was separated. Then, this oil layer was distilled to recover 28.5 g of triethylamine, and then 32.3 g (purity: 99%, yield: 91.0%) of 3,5-difluoroaniline was obtained.

1. customThen, the mixture was reacted under a hydrogen gas pressure of 15 kg/cm2 at a temperature of 100° C. for 4 hours
2. filtrationThen, palladium-carbon was filtered off
3. addition50 g of a 25% sodium hydroxide aqueous solution was added
4. waitleft
5. customThen, the oil layer was separated
6. distillationThen, this oil layer was distilled
7. customto recover 28.5 g of triethylamine