HRID1013914

反应详情

EQUATION

反应方程式

HRID 1013914 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 6.59 g (0.025 moles) of the 4-benzyloxy-3-chloro nitrobenzene (example 4), 4.19 g (0.075 moles) of iron powder, and 12.04 g (0.225 moles) of ammonium chloride in 100 ml of ethanol and 25 ml of water was stirred mechanically and refluxed for half an hour. The reaction was allowed to cool and stir for 1 hour. The mixture was filtered and solids were washed with ethanol. The combined filtrates were taken to dryness in vacuo. This solid was dissolved in methylene chloride and passed through Magnesol. Removal of the solvent from the filtrate in vacuo gave 5.60 g of title compound.

WORKUP

后处理

  1. temperaturerefluxed for half an hour
  2. temperatureto cool
  3. stirringstir for 1 hour
  4. filtrationThe mixture was filtered
  5. washsolids were washed with ethanol
  6. dissolutionThis solid was dissolved in methylene chloride
  7. customRemoval of the solvent from the filtrate in vacuo