反应详情

Bromine (4.8 g) was added in one portion to a mixture of 5-amino-2-methoxy-4-methylpyridine (3.9 g) in acetic acid (25 ml) and sodium acetate (4.0 g). The resulting mixture was stirred for 20 min. and then added to a solution of sodium hydroxide (15 g) in water (200 ml). The product was extracted with chloroform, dried (anhydrous magnesium sulfate), concentrated, and purified on a silica gel column (methylene chloride/ethyl acetate, 19:1→4:1) to give 4.5 g of the title compound, suitable for use in the next reaction.

1. extractionThe product was extracted with chloroform
2. dry with materialdried (anhydrous magnesium sulfate)
3. concentrationconcentrated
4. custompurified on a silica gel column (methylene chloride/ethyl acetate, 19:1→4:1)