HRID606116

反应详情

EQUATION

反应方程式

HRID 606116 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-{2-[3-(4-fluorophenyl)isoxazol-5-yl]ethyl}-1H-isoindole-1,3(2H)-dione (27.14 g, 80.70 mmol), hydrazine hydrate (9.8 mL, 202 mmol), and ethanol (700 mL) was heated at reflux under nitrogen for two hours. The reaction mixture was filtered to remove a solid, and the filtrate was concentrated under reduced pressure. The resulting oil was dissolved in ethyl acetate, and the solution was washed sequentially with water and brine, dried over sodium sulfate, filtered, and concentrated under reduced pressure to provide 16.14 g of 2-[3-(4-fluorophenyl)isoxazol-5-yl]ethylamine as a colorless oil.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux under nitrogen for two hours
  3. filtrationThe reaction mixture was filtered
  4. customto remove a solid
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. dissolutionThe resulting oil was dissolved in ethyl acetate
  7. washthe solution was washed sequentially with water and brine
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure