HRID56002

反应详情

EQUATION

反应方程式

HRID 56002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To 111 mg of N-[2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-2-(ethoxyimino)ethyl]phthalimide in 3 ml of ethanol, 86 mg of hydrazine monohydrate was added, and the mixture was stirred at 80° C. for 1 hour. After completion of the reaction, the reaction mixture was allowed to cool to room temperature, mixed with 5 ml of water and extracted with ethyl acetate (5 ml×3). The resulting organic layers were combined, dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and the resulting residue was purified by silica gel column chromatography using methanol-chloroform (1:10) as the eluent to obtain 47 mg of the desired product as a yellow oil. The oil was used in the next step without further purification.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. temperatureto cool to room temperature
  3. extractionextracted with ethyl acetate (5 ml×3)
  4. dry with materialdried over saturated aqueous sodium chloride
  5. customanhydrous sodium sulfate, the solvent was evaporated under reduced pressure
  6. customthe resulting residue was purified by silica gel column chromatography