反应详情

To a solution of 2-methoxy-6-methylbenzonitrile (3.6 g, 24 mmol) in TFA (25 mL) was added NBS (6.5 g, 36 mmol) and stirred at room temperature for 2 hours. Analysis of the reaction mixture by LC indicated complete bromination of the starting material. The solution was concentrated in vacuo and the resulting crude was dissolved in EtOAc and washed with brine, then dried with Na2SO4, filtered and concentrated in vacuo. The crude residue was purified by silica gel column chromatography (Hexanes:EtOAc=1:1) to provide the title product.

1. concentrationThe solution was concentrated in vacuo
2. dissolutionthe resulting crude was dissolved in EtOAc
3. washwashed with brine
4. dry with materialdried with Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe crude residue was purified by silica gel column chromatography (Hexanes:EtOAc=1:1)