HRID276707

反应详情

EQUATION

反应方程式

HRID 276707 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-[1-(cyanomethyl-carbamoyl)-cyclohexyl]-4-bromomethyl-benzamide (0.34 mmol) is dissolved in THF (2 ml) and sodium-imidazol (0.41 mmol) is added and the reaction mixture stirred at RT over night. After evaporation of the solvent, the residue is extracted with ethyl acetate. The extract is washed with water, dried over magnesium sulfate and evaporated. The residue was suspended in diethylether and the solid filtered of. The crude product is purified by chromatography on silica using CH2Cl2/MeOH=9:1. The fractions containing the pure product were collected and evaporated. The residue was suspended in diethylether and the solid filtered of. A white powder with mp. 194-196° C., Rf=0.28 (CH2Cl2/MeOH=9:1) is obtained.

WORKUP

后处理

  1. customAfter evaporation of the solvent
  2. extractionthe residue is extracted with ethyl acetate
  3. washThe extract is washed with water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. filtrationthe solid filtered of
  7. customThe crude product is purified by chromatography on silica
  8. additionThe fractions containing the pure product
  9. customwere collected
  10. customevaporated
  11. filtrationthe solid filtered of
  12. customA white powder with mp. 194-196° C., Rf=0.28 (CH2Cl2/MeOH=9:1) is obtained