HRID1017655

反应详情

EQUATION

反应方程式

HRID 1017655 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureat reflux overnight
  2. washthe reaction mixture was washed with ether
  3. customthe aqueous layer was separated
  4. extractionThe product was extracted into ethyl acetate
  5. dry with materialdried over potassium carbonate/sodium carbonate
  6. concentrationconcentrated
  7. customThe residue was purified by flash chromatography (5% methanol/methylene chloride gradient)