反应详情

To 30 ml of toluene were added 5-chlorosalicylic acid (862 mg, 5 mmol), 3,5-bis(trifluoromethyl)aniline (1.37 g, 6 mmol), and phosphoroustrichloride (755 mg, 5.5 mmol) in the presence of argon gas, followed by stirring for 6 hours through heat-reflux. Sodium hydrogen carbonate was added to the mixture to adjust pH to 7, followed by concentration under reduced pressure. The mixture was dissolved in 60 ml of ethylacetate, which was washed with water (40 ml×2). The organic layer was concentrated under reduced pressure, followed by column chromatography to give 1.09 g of the target compound (yield: 57%).

1. temperaturethrough heat-reflux
2. concentrationfollowed by concentration under reduced pressure
3. dissolutionThe mixture was dissolved in 60 ml of ethylacetate
4. washwhich was washed with water (40 ml×2)
5. concentrationThe organic layer was concentrated under reduced pressure