HRID653473

反应详情

EQUATION

反应方程式

HRID 653473 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.35 g of 5% palladium-on-carbon catalyst is added to a solution of 3.5 g of 1-(4-nitrophenyl)-3-n-propyl-3-azabicyclo[3.1.1]heptane-2,4-dione in 70 ml of ethyl acetate and the whole is hydrogenated under normal pressure and at 30°-35° in a hydrogen atmosphere. When the absorption of hydrogen is complete, the reaction mixture is diluted with 30 ml of methylene chloride and freed of catalyst by filtration over HYFLO Super-Cel®. The solvent is evaporated off in vacuo, and the residue is recrystallised from a mixture of ethyl acetate/n-hexane, yielding the title compound in the form of white crystals having a melting point of 166°-167°.

WORKUP

后处理

  1. customWhen the absorption of hydrogen
  2. additionthe reaction mixture is diluted with 30 ml of methylene chloride
  3. filtrationfreed of catalyst by filtration over HYFLO Super-Cel®
  4. customThe solvent is evaporated off in vacuo
  5. customthe residue is recrystallised from a mixture of ethyl acetate/n-hexane