HRID6754
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
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
Phosphorus oxychloride (22.5 mL) was added to a solution of N-[2-(4-methoxy-phenyl)-ethyl]-acetamide (6.5 g) in acetonitrile (200 mL). The mixture was heated at 120° C. in a sealed tube for 16 h. The solvent was evaporated. The residue was dissolved in dichloromethane (200 mL) and washed with aqueous sodium bicarbonate (saturated, 100 mL) and brine (100 mL). The dichloromethane layer was dried over sodium sulfate, filtered and evaporated. The crude product was purified by column chromatography (5% methanol in dichloromethane) to afford 7-methoxy-1-methyl-3,4-dihydro-isoquinoline (2.67 g).
WORKUP
后处理
- customThe solvent was evaporated
- dissolutionThe residue was dissolved in dichloromethane (200 mL)
- washwashed with aqueous sodium bicarbonate (saturated, 100 mL) and brine (100 mL)
- dry with materialThe dichloromethane layer was dried over sodium sulfate
- filtrationfiltered
- customevaporated
- customThe crude product was purified by column chromatography (5% methanol in dichloromethane)