反应详情

A mixture of 6-methyl-pyridine-2-carboxylic acid ethyl ester (1.65 g, 10 mmol), NBS (1.77 g, 10 mmol), and benzoyl peroxide (100 mg) in carbon tetrachloride (20 ml) was refluxed for 14 h. After cooling to room temperature, the reaction mixture was partitioned between diethyl ether and water (120 ml, 4:1), organic layer was washed with water (2×20 ml), brine, dried (MgSO4), filtered and concentrated to give 6-bromomethyl-pyridine-2-carboxylic acid ethyl ester (2.4 g) which was used without further purification. LCMS m/z: 245 (M+1)+.

1. temperaturewas refluxed for 14 h
2. customthe reaction mixture was partitioned between diethyl ether and water (120 ml, 4:1), organic layer
3. washwas washed with water (2×20 ml), brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated