HRID1773559
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
A mixture of 7-methoxy-6-nitro-quinoline (5 g, 24.0 mmol), iron powder (9.8 g, 172 mmol) and ammonium chloride (9.1 g, 172 mmol) in a mixture of ethanol and water (3/1, 160 mL) was heated at reflux overnight. The resulting mixture was filtered through a CELITE™ pad, the filtrate was evaporated under reduced pressure and the residue was partitioned between water and ethyl acetate. The organic layer was separated, dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified by flash chromatography (EtOAc) to afford 3.551 g of 7-methoxy-quinolin-6-ylamine as a grey solid.
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux overnight
- filtrationThe resulting mixture was filtered through a CELITE™ pad
- customthe filtrate was evaporated under reduced pressure
- customthe residue was partitioned between water and ethyl acetate
- customThe organic layer was separated
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- customevaporated under reduced pressure
- customThe residue was purified by flash chromatography (EtOAc)