HRID466369

反应详情

EQUATION

反应方程式

HRID 466369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 0.46 g (1.35 mmol) of the ketoamine free base, N-[4-[2-(Dibutylamino)-1-oxoethyl]phenyl]methanesulfonamide, 0.15 g of 10% palladium on carbon catalyst and 150 ml of absolute EtOH is placed on a Parr hydrogenator and shaken under an hydrogen atmosphere for 18.5 hrs. The catalyst is removed by filtration and the filtrate is concentrated in vacuo. The residue is chromatographed on a 100 ml silica gel column (elution with 3% MeOH:CH2Cl2 containing 0.3% NH4OH) and fractions are collected. The title compound is recrystallized from Et2O:pet. ether.

WORKUP

后处理

  1. customThe catalyst is removed by filtration
  2. concentrationthe filtrate is concentrated in vacuo
  3. customThe residue is chromatographed on a 100 ml silica gel column (elution with 3% MeOH:CH2Cl2 containing 0.3% NH4OH) and fractions
  4. customare collected
  5. customThe title compound is recrystallized from Et2O