HRID648636

反应详情

EQUATION

反应方程式

HRID 648636 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Five milliliters of 1N sodium hydroxide solution were added to a solution of 0.85 gm (1.7 m mol) of 4-[(1-(2-piperidino-phenyl)-ethyl)-aminocarbonylmethyl]-benzyl malonic acid diethyl ester in 18 ml of ethanol. After stirring for two hours at 50° C., the mixture was evaporated in vacuo, and water and 5 ml of 1N hydrochloric acid were added. The precipitate formed was filtered off, dried in vacuo, and heated for 30 minutes up to 120° C., whereby carbon dioxide was split off. The product obtained was purified by column chromatography on silica gel (chloroform/methanol=20:1).

WORKUP

后处理

  1. customthe mixture was evaporated in vacuo, and water and 5 ml of 1N hydrochloric acid
  2. additionwere added
  3. customThe precipitate formed
  4. filtrationwas filtered off
  5. customdried in vacuo
  6. temperatureheated for 30 minutes up to 120° C., whereby carbon dioxide
  7. customwas split off
  8. customThe product obtained
  9. customwas purified by column chromatography on silica gel (chloroform/methanol=20:1)