反应详情

To tert-butyl-(2,4-difluoro-phenoxy)-dimethyl-silane (36, 5.90 g, 24.1 mmol) in tetrahydrofuran (100 mL), under an atmosphere of nitrogen, cooled in a −78° C. acetone/dry ice bath, was added n-butyllithium (2.50 M in hexane, 10.6 mL, 26.5 mmol) slowly. The reaction was allowed to stir for 1 hour, then N,N-dimethylformamide (2.24 mL, 29.0 mmol) was added and the reaction was allowed to warm to room temperature overnight. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate and concentrated. The compound was isolated by silica gel column chromatography eluting with 10% ethyl acetate in hexane to give a colorless oil (37, 5.0 g, 76.0%). MS (ESI) [M+H+]+=272.2.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated
5. customThe compound was isolated by silica gel column chromatography
6. washeluting with 10% ethyl acetate in hexane
7. customto give a colorless oil (37, 5.0 g, 76.0%)