反应详情

To dibenzyl-(2,4-difluoro-phenyl)-amine (3.097 g, 10.02 mmol) in tetrahydrofuran (45 mL), under nitrogen atmosphere, cooled at −78° C. acetone/dry in ice bath, n-butyllithium (1.6 M in hexane, 6.88 mL, 11.02 mmol) was added slowly. The reaction was stirred for 1 hour, benzyl chloroformate (1.54 mL, 11.02 mmol) was added and the reaction was allowed to warm to room temperature during 2 hours. The reaction was poured into water and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and purified by silica gel column chromatography eluting with 5% ethyl acetate in hexane grading to 10% acetate to provide the title compound as colourless oil (4.0 g, 90%).

1. customdry in ice bath
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationThe filtrate was concentrated
7. custompurified by silica gel column chromatography
8. washeluting with 5% ethyl acetate in hexane grading to 10% acetate