反应详情

To 300 ml of a solution of 65.0 g (301 mmol) of 2-bromo-5-methylnitrobenzene in tetrahydrofuran was added 1 liter of a 1.0 M solution of vinyl magnesium bromide (1 mol) in tetrahydrofuran at −60° C. in a nitrogen atmosphere under stirring during 1 hour. To the reaction mixed solution were added a saturated aqueous solution of ammonium chloride and ethyl acetate, and the resulting insoluble matters were filtered off. The resulting filtrate was dried over magnesium sulfate, concentrated, and then the resulting residue was purified by a silica gel column chromatography to give 35.5 g of the title compound.

1. additionTo the reaction mixed solution
2. filtrationthe resulting insoluble matters were filtered off
3. dry with materialThe resulting filtrate was dried over magnesium sulfate
4. concentrationconcentrated
5. customthe resulting residue was purified by a silica gel column chromatography