HRID622679

反应详情

EQUATION

反应方程式

HRID 622679 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of piperid-4-one oxime (46 g; 0.04 moles), 2-tetrahydrofurylmethyl methanesulphonate (79.3 g; 0.44 moles) and anhydrous potassium carbonate (56.5 g; 0.40 moles) in methyl isobutyl ketone (625 ml), was boiled under reflux with stirring for 48 hours. After cooling, the reaction mixture was washed with brine, dried (Na2SO4), and the solvent removed in vacuo. The residue was crystallised from diisopropyl ether to give 1-(2-tetrahydrofurylmethyl)-piperid-4-one oxime (42.5 g), m.p. 104°-106°.

WORKUP

后处理

  1. temperatureunder reflux
  2. temperatureAfter cooling
  3. washthe reaction mixture was washed with brine
  4. dry with materialdried (Na2SO4)
  5. customthe solvent removed in vacuo
  6. customThe residue was crystallised from diisopropyl ether