HRID1270080

反应详情

EQUATION

反应方程式

HRID 1270080 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a well stirred suspension of (0.05 mol) of lithium alumunium hydride in 100 ml of anhydrous tetrahydrofuran, (0.043 mole) of 1-(2-cyanophenyl)pyrrole were added by small portions. Then the mixture was maintained with stirring at room temperature for 18 hours. Addition of aqueous ethanol to destroy the excess lithium aluminium hydride, followed by filtration afforded a solution, which was then evaporated in vacuo. The residue was extracted with ethyl ether, the organic layer washed with water and dried over anhydrous sodium sulphate. Removal of the solvent under reduced pressure gave a crude product, which was purified by passing through an alumina column eluting with chloroform to give 1-(2-aminomethylphenyl)pyrrole.

WORKUP

后处理

  1. additionwere added by small portions
  2. temperatureThen the mixture was maintained
  3. stirringwith stirring at room temperature for 18 hours
  4. customto destroy the excess lithium aluminium hydride
  5. filtrationfollowed by filtration
  6. customafforded a solution, which
  7. customwas then evaporated in vacuo
  8. extractionThe residue was extracted with ethyl ether
  9. washthe organic layer washed with water
  10. dry with materialdried over anhydrous sodium sulphate
  11. customRemoval of the solvent under reduced pressure
  12. customgave a crude product, which
  13. customwas purified
  14. washeluting with chloroform