反应详情

温度

80 °C

A mixture of 3,5-bis(trifluoromethyl)aniline (0.20 g, 0.87 mmol), N-(tert-butoxycarbonyl)-L-phenylalanine (254.8 mg, 0.96 mmol), phosphorus trichloride (40 μL, 0.46 mmol) and toluene (4 mL) was stirred at 80° C. for 1.5 hours under argon atmosphere. After the reaction mixture was cooled to room temperature, it was poured into aqueous sodium hydrogen carbonate and extracted with ethyl acetate. After the ethyl acetate layer was washed with brine, dried over anhydrous sodium sulfate, the residue obtained by evaporation of the solvent under reduced pressure was crystallized by isopropyl ether/n-hexane to give the title compound (333.7 mg, 92.9%) as an yellow white powder.

1. temperatureAfter the reaction mixture was cooled to room temperature
2. extractionextracted with ethyl acetate
3. washAfter the ethyl acetate layer was washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. customthe residue obtained by evaporation of the solvent under reduced pressure
6. customwas crystallized by isopropyl ether/n-hexane