HRID1017655
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 solution of N-[3-(4-fluorobenzoyl)pyridin-4-yl]-2,2-dimethylpropanamide (2.85 g, 9.5 mmol) in 3 N aqueous HCl (15 ml) was warmed at reflux overnight. After cooling to room temperature, the reaction mixture was washed with ether, the aqueous layer was separated and neutralized with potassium carbonate. The product was extracted into ethyl acetate, dried over potassium carbonate/sodium carbonate and concentrated. The residue was purified by flash chromatography (5% methanol/methylene chloride gradient) to afford 4-amino-3-(4-fluorobenzoyl)pyridine (1.58 g).
WORKUP
后处理
- temperatureat reflux overnight
- washthe reaction mixture was washed with ether
- customthe aqueous layer was separated
- extractionThe product was extracted into ethyl acetate
- dry with materialdried over potassium carbonate/sodium carbonate
- concentrationconcentrated
- customThe residue was purified by flash chromatography (5% methanol/methylene chloride gradient)