HRID253966

反应详情

EQUATION

反应方程式

HRID 253966 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of the N-tert-butyl-3-nitropyridin-2-amine in MeOH (200 mL), was added solid NH4Cl (16.4 g, 306.54 mmol) and zinc dust (10.0 g, 153 mmol). The suspension was heated under reflux for 3 hours and then cooled to RT. After filtration through Celite™, the solvent was removed by vacuum evaporation. The resulting black residue was taken up to EtOAc (300 mL) and filtered through Celite™ again to remove the remaining NH4Cl. The solvent was again evaporated and the residue was dried on the high vacuum oil pump overnight to yield N2-tert-butylpyridine-2,3-diamine.

WORKUP

后处理

  1. temperatureThe suspension was heated
  2. temperatureunder reflux for 3 hours
  3. filtrationAfter filtration through Celite™
  4. customthe solvent was removed by vacuum evaporation
  5. filtrationfiltered through Celite™ again
  6. customto remove the remaining NH4Cl
  7. customThe solvent was again evaporated
  8. customthe residue was dried on the high vacuum oil