HRID1005491

反应详情

EQUATION

反应方程式

HRID 1005491 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.5 g of 2,3-difluoro-6-trifluoromethylbenzaldehyde in 8 ml of ethanol was added 0.4 g of hydroxylamine hydrochloride and a solution prepared by dissolving 0.23 g of sodium hydroxide into 2 ml of water and the mixture was heated at reflux for 40 minutes. The reaction mixture was allowed to room temperature, then concentrated under reduced pressure and extracted with ethyl acetate. The extract obtained was washed with water and with saturated saline solution and dried over anhydrous magnesium sulfate. After concentrating the extract solution, the crude product obtained was washed with n-hexane to obtain 0.24 g of the title compound (mp. 111-112° C.).

WORKUP

后处理

  1. customa solution prepared
  2. temperaturethe mixture was heated
  3. temperatureat reflux for 40 minutes
  4. customwas allowed to room temperature
  5. concentrationconcentrated under reduced pressure
  6. extractionextracted with ethyl acetate
  7. customThe extract obtained
  8. washwas washed with water and with saturated saline solution
  9. dry with materialdried over anhydrous magnesium sulfate
  10. concentrationAfter concentrating the extract solution
  11. customthe crude product obtained
  12. washwas washed with n-hexane