HRID1865284

反应详情

EQUATION

反应方程式

HRID 1865284 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Ethyl-1-benzyl-3-methyl-4-oxo-piperidine-3-carboxylate (85 g, 0.31 mol) was dissolved in conc HCl (82 ml, 0.77 mol) and the reaction mixture was heated to 100° C. for 32 hrs. Solvent was removed under reduced pressure and the resulting solid was dissolved in the 300 ml CHCl3 and 400 ml pet ether was added to this under stirring to provide a solid. The solid was filter and was dissolved in 400 ml ethyl acetate and organic layer was washed with 10% NaOH aqueous solution. Layers were separated and concentration of organic layer afforded 48 g (75%) oil as a titled product.

WORKUP

后处理

  1. customSolvent was removed under reduced pressure
  2. dissolutionthe resulting solid was dissolved in the 300 ml CHCl3 and 400 ml pet ether
  3. additionwas added to
  4. customto provide a solid
  5. filtrationThe solid was filter
  6. dissolutionwas dissolved in 400 ml ethyl acetate
  7. washorganic layer was washed with 10% NaOH aqueous solution
  8. customLayers were separated