反应详情

To a stirred solution of 4-Bromo-3-fluoro-N-methoxy-N-methylbenzamide (3.0 g, 12.19 mmol) in tetrahydrofuran (35 ml) was added 2M n-propylmagnesium bromide (12.2 ml, 24.38 mmol) dropwise under nitrogen at 0° C. The reaction mixture was stirred at room temperature for 2 h. This was quenched by sat. ammonium chloride and stirred at rt for 30 min. The organic layer was separated and the aqueous layer was extracted with ethyl acetate. The extracts was dried (MgSO4) and concentrated. This was purified on silica gel eluting with ethyl acetate/hexane (1:10) to afford 2.44 g (81.7%) of the titled compound as a slight yellow oil.

1. customThis was quenched by sat. ammonium chloride
2. stirringstirred at rt for 30 min
3. customThe organic layer was separated
4. extractionthe aqueous layer was extracted with ethyl acetate
5. dry with materialThe extracts was dried (MgSO4)
6. concentrationconcentrated
7. customThis was purified on silica gel eluting with ethyl acetate/hexane (1:10)