HRID641806
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 2-methyl-6-nitroquinoline (12 g, 63.84 mmol) in HCl (1N, 450 mL) was added a solution of SnCl2.2H2O (72 g, 0.32 mol) in HCl (1N, 150 mL) slowly. The reaction mixture was heated to reflux for 15 min, then cooled to room temperature. The precipitate was filtered. The filtrate was basified by aqueous KOH and extracted with EtOAc. The organic layer was dried over anhydrous Na2SO4 and the solvent was removed under reduced pressure to give 6.9 g of 2-methylquinolin-6-amine (68.3%). MS [M++1]=159, LC-MS: tR=0.255 min.
WORKUP
后处理
- temperatureThe reaction mixture was heated
- temperatureto reflux for 15 min
- filtrationThe precipitate was filtered
- extractionextracted with EtOAc
- dry with materialThe organic layer was dried over anhydrous Na2SO4
- customthe solvent was removed under reduced pressure