HRID977087

反应详情

EQUATION

反应方程式

HRID 977087 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

500 mg of N-(1-adamantyl)-3-(3-nitro-4-aminophenyl)propionamide (prepared as described in Example 21) was dissolved in 20 ml of methanol. 200 mg of 10% w/w palladium-on-carbon was added to the solution, which was then catalytically reduced whilst bubbling hydrogen through it, under atmospheric pressure for 120 minutes. The catalyst was then removed by filtration, and the methanol was removed by distillation under reduced pressure. The resulting residue was purified by silica gel column chromatography, using 19:1 ethyl acetate:methanol as the eluent, to afford 0.21 g of the title compound as crystals, melting at 151°-152° C.

WORKUP

后处理

  1. customwhilst bubbling hydrogen through it
  2. customThe catalyst was then removed by filtration
  3. customthe methanol was removed by distillation under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography