反应详情

To 2,4-difluoroaniline (40.0 g, 0.31 mol) in N,N-dimethylformamide (400 mL) were added potassium carbonate (120 g, 0.92 mol, 3 eq) and benzyl bromide (112 mL, 0.71 mmol, 2.3 eq). The reaction was stirred with mechanical stirring at room temperature overnight. In order to quench the benzyl bromide in excess, NH4OH (90 mL) was added and the reaction was stirred overnight. The mixture was filtered and DMF was evaporated under reduced pressure. Ethyl acetate was added and the organic layer was washed with water and brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under reduced pressure and the oily crude was crystallized in methanol, obtaining after drying 71 g of dibenzyl-(2,4-difluoro-phenyl)-amine as a white solid (74%)

1. stirringwith mechanical stirring at room temperature overnight
2. customIn order to quench the benzyl bromide in excess, NH4OH (90 mL)
3. additionwas added
4. stirringthe reaction was stirred overnight
5. filtrationThe mixture was filtered
6. customDMF was evaporated under reduced pressure
7. additionEthyl acetate was added
8. washthe organic layer was washed with water and brine
9. dry with materialdried over anhydrous sodium sulfate
10. filtrationfiltered
11. concentrationThe filtrate was concentrated under reduced pressure
12. customthe oily crude was crystallized in methanol
13. customobtaining
14. dry with materialafter drying 71 g of dibenzyl-(2,4-difluoro-phenyl)-amine as a white solid (74%)