HRID728323

反应详情

EQUATION

反应方程式

HRID 728323 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 25.03 g (100 mole) of 2-nicotinoylaminoethyl acetoacetate, 15.11 g (100 mmole) of m-nitrobenzaldehyde and 15.42 g (100 mmole) of 2-cyanoethyl 3-aminocrotonate in 150 ml of isopropyl alcohol was added 0.73 g (5 mmole) of piperidinium acetate, and the mixture was refluxed for 5 hours. After evaporation of the solvent, the residue was dissolved in 200 ml of acetone. To the solution was added 200 ml of 0.75 N aqueous sodium hydroxide solution, and the mixture was stirred at room temperature for an hour. 1N hydrochloric acid was added, and the solution was concentrated and extracted with chloroform Evaporation of the solvent gave 45.27 g of 2,6-dimethyl4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid 3-(2-nicotinoylaminoethyl) ester.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 5 hours
  2. customAfter evaporation of the solvent
  3. dissolutionthe residue was dissolved in 200 ml of acetone
  4. additionTo the solution was added 200 ml of 0.75 N aqueous sodium hydroxide solution
  5. addition1N hydrochloric acid was added
  6. concentrationthe solution was concentrated
  7. extractionextracted with chloroform Evaporation of the solvent