HRID477178

反应详情

EQUATION

反应方程式

HRID 477178 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

12 Grams of 2-nitro-5-chlorobenzaldehyde dimethyl acetal, 16.3 g of 4-acetylaminopiperidine hydrochloride, 13.7 g of sodium carbonate and 13 ml of triethylamine in 150 ml of N-methylpyrrolidone solution were mixed together and reacted by heating at 120° C. for 12 hours with stirring under nitrogen gas stream. After the reaction was completed, the solvent was removed by evaporation and thus obtained residue was added with water and extracted with dichloromethane, then the extract was washed with water and with an aqueous solution saturated with sodium chloride, then dried with anhydrous sodium sulfate. The solvent was removed by evaporation and the residue thus obtained was added with diethyl ether, then the crystals formed were collected by filtration to yield 11.2 g of 2-nitro-5-(4-acetylamino-1-piperidyl)benzaldehyde dimethylacetal.

WORKUP

后处理

  1. customreacted
  2. customthe solvent was removed by evaporation and thus obtained residue
  3. additionwas added with water
  4. extractionextracted with dichloromethane
  5. washthe extract was washed with water and with an aqueous solution saturated with sodium chloride
  6. dry with materialdried with anhydrous sodium sulfate
  7. customThe solvent was removed by evaporation
  8. customthe residue thus obtained
  9. customthe crystals formed
  10. filtrationwere collected by filtration