HRID1246062

反应详情

EQUATION

反应方程式

HRID 1246062 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-(4-aminomethylphenyl)-4-nitroanisole (4.50 g) in methanol (200 mL) was treated with 10% palladium on carbon (200 mg). The reaction mixture was stirred under one atmosphere of hydrogen for 2.5 hours. The reaction mixture filtered through Celite, and the filter cake was washed with methanol (3×25 mL). The filtrate was concentrated to dryness and the residue was purified by flash chromatography on silica gel (80 g) eluting with 0–6% methanol/0.5% triethylamine/dichloromethane. Pure fractions were combined and concentrated to give 3-(4-aminomethylphenyl)-4-methoxyaniline as an off white powder.

WORKUP

后处理

  1. filtrationThe reaction mixture filtered through Celite
  2. washthe filter cake was washed with methanol (3×25 mL)
  3. concentrationThe filtrate was concentrated to dryness
  4. customthe residue was purified by flash chromatography on silica gel (80 g)
  5. washeluting with 0–6% methanol/0.5% triethylamine/dichloromethane
  6. concentrationconcentrated