HRID67120

反应详情

EQUATION

反应方程式

HRID 67120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7.8 gm (0.03 mol) of 1-[2-cyano-4-(isobutyroyl-amino)-phenoxy]-2,3-epoxy-propane were dissolved in 80 ml of ethanol, and after addition of 7.5 gm (0.06 mol) of 1-ethinyl-cyclohexyl-amine the mixture was refluxed for one hour. The solvent was then distilled off, and the residue was acidified with dilute HCl. After extraction with ethyl acetate the aqueous phase was made alkaline by addition of NaOH, whereby basic components precipitated in oily form. They were taken up in ethyl acetate, the organic phase was washed with water, dried over MgSO4, evaporated and the solid residue was recrystallized twice from acetonitrile.

WORKUP

后处理

  1. temperaturewas refluxed for one hour
  2. distillationThe solvent was then distilled off
  3. extractionAfter extraction with ethyl acetate the aqueous phase
  4. additionby addition of NaOH, whereby basic components
  5. customprecipitated in oily form
  6. washthe organic phase was washed with water
  7. dry with materialdried over MgSO4
  8. customevaporated
  9. customthe solid residue was recrystallized twice from acetonitrile