HRID1354869

反应详情

EQUATION

反应方程式

HRID 1354869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. filtrationThe reaction mixture was filtered over HFLO
  2. concentrationconcentrated under reduced pressure to 5 mL
  3. additionDichloromethane (100 mL) was added
  4. washthe resultant solution was washed with water
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated