HRID862061
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 2-(5-bromo-2-methoxymethoxybenzoyl)-3-methoxymethoxypyridine (1.89 g), hydrochloric acid (10 ml) and methanol (80 ml) was stirred for 70 hours at room temperature. The reaction mixture was concentrated, which was partitioned with ethyl acetate-water. The organic layer was washed with a saturated aqueous saline solution, dried (anhydrous sodium sulfate) and concentrated. The concentrate was purified by means of a silica gel column chromatography (eluted with ethyl acetate/hexane) to give 2-(5-bromo-2-hydroxybenzoyl)-3-hydroxypyridine (1.34 g) (Compound A-1).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- customwhich was partitioned with ethyl acetate-water
- washThe organic layer was washed with a saturated aqueous saline solution
- dry with materialdried (anhydrous sodium sulfate)
- concentrationconcentrated
- customThe concentrate was purified by means of a silica gel column chromatography (eluted with ethyl acetate/hexane)