HRID1354869
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 1.5 g (8.37 mmol) of 4-nitrocinnamyl alcohol in THF/methanol (60 mL, 1:1 v/v) was added a catalytic amount of Raney Nickel and hydrazine monohydrate (1.22 mL, 25.1 mmol). The mixture was stirred at room temperature for 3 h, additional hydrazine monohydrate (1.22 mL) being added after 1.5 h. The reaction mixture was filtered over HFLO and concentrated under reduced pressure to 5 mL. Dichloromethane (100 mL) was added and the resultant solution was washed with water, dried over Na2SO4, filtered, and concentrated, which gave 10 (1.24 g, 8.31 mmol, 99%).
WORKUP
后处理
- filtrationThe reaction mixture was filtered over HFLO
- concentrationconcentrated under reduced pressure to 5 mL
- additionDichloromethane (100 mL) was added
- washthe resultant solution was washed with water
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated