HRID1520182

反应详情

EQUATION

反应方程式

HRID 1520182 的结构方程式

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To the solid of 3-chloro-N-(3-fluorophenyl)propanamide (3 g, 14.88 mmol) was added AlCl3 (6.3 g, 0.047 mmol) and maintained with an inert atmosphere of nitrogen with stirring for 5 h at 120° C. The reaction was then quenched with ice-water, extracted with ethyl acetate (3×50 ml) and the organic layers were combined, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography with 4% ethyl acetate in petroleum ether to afford 7-fluoro-1,2,3,4-tetrahydroquinolin-2-one as a white solid (1.5 g, 61%).

WORKUP

后处理

  1. temperaturemaintained with an inert atmosphere of nitrogen
  2. customThe reaction was then quenched with ice-water
  3. extractionextracted with ethyl acetate (3×50 ml)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by silica gel column chromatography with 4% ethyl acetate in petroleum ether