反应详情

To a solution of 75.5 g 5-ethoxy-2-fluoro-phenol described in example 1.1 in 250 ml DMA were added 80.2 g t-butyl dimethylchlorsilane and 36.2 g imidazole at 0° C. The reaction mixture was warmed to r.t. After 4 hrs, 400 ml water were added. The mixture was extracted with hexane. The organic layer was washed with water, 10% Na2CO3 solution, water and brine, dried over MgSO4, filtrated and concentrated to give 127.0 g tert-butyl-(5-ethoxy-2-fluoro-phenoxy)-dimethyl-silane as light brown liquid which was used in the next step without further purification.

1. extractionThe mixture was extracted with hexane
2. washThe organic layer was washed with water, 10% Na2CO3 solution, water and brine
3. dry with materialdried over MgSO4
4. filtrationfiltrated
5. concentrationconcentrated