反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
Under nitrogen, to the slurry of lithium aluminum hydride (11.4 g) in tetrahydrofuran (200 ml) was added 6-methoxy-1-(trimethylsilanyloxy)-1,2,3,4-tetrahydronaphthalene-1-carbonitrile (41.3 g) in tetrahydrofuran (200 ml) dropwise at 5° C., and the mixture was stirred at the same temperature for 1 hour and at room temperature for 2 hours. To the mixture were added sodium fluoride (12.6 g) and water (16.2 ml) at 5° C., and the mixture was vigorously stirred at room temperature for 30 minutes. The precipitate was removed by filtration and the filter cake was washed with ethyl acetate-ethanol (95:5). The filtrate was evaporated in vacuo to afford 1-aminomethyl-5-methoxy-1,2,3,4-tetrahydronaphthalen-1-ol (28.6 g).
WORKUP
后处理
- stirringthe mixture was vigorously stirred at room temperature for 30 minutes
- customThe precipitate was removed by filtration
- washthe filter cake was washed with ethyl acetate-ethanol (95:5)
- customThe filtrate was evaporated in vacuo