HRID30530
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
- -78 °C
PROCEDURE
实验过程
Next, to a flask containing a mixture of 7-ethoxy-naphthalen-1-ylamine (1.80 g, 9.61 mmol) and t-butanol (2.13 g, 28.8 mmol) in tetrahydrofuran (20 mL) was collected liquid ammonia (300 mL) at −78° C. To the mixture was added lithium (0.200 g, 28.8 mmol) over 30 minutes and stirred at −78° C. for 1 hour. Methanol and water was added, and the mixture was stirred at room temperature for 16 hours to allow ammonia to evaporate. To the obtained residue was added ethyl acetate. The organic layer was washed with water, dried over Na2SO4, filtered, and concentrated under reduced pressure to afford 7-ethoxy-5,8-dihydronaphthalen-1-ylamine (1.37 g, 76% yield).
WORKUP
后处理
- additionNext, to a flask containing
- customwas collected liquid ammonia (300 mL) at −78° C
- stirringthe mixture was stirred at room temperature for 16 hours
- customto evaporate
- additionTo the obtained residue was added ethyl acetate
- washThe organic layer was washed with water
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure