HRID1518520
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe suspension was heated
- temperatureunder reflux for 3 hours
- filtrationAfter filtration through Celite™
- customthe solvent was removed by vacuum evaporation
- filtrationfiltered through Celite™ again
- customto remove the remaining NH4Cl
- customThe solvent was again evaporated
- customthe residue was dried on the high vacuum oil