HRID727806

反应详情

EQUATION

反应方程式

HRID 727806 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

117.8 g (0.42 mol) of 2-(4-nitrophenoxymethyl)quinoline were dissolved in 1 l of methanol/tetrahydrofuran (1:1). About 5 g of Raney nickel were then added and the mixture was warmed to 35° C. 63.1 g (1.26 mol) of hydrazine hydrate ×H2O were then added dropwise and the mixture was stirred overnight. The residue was filtered off, the solution was concentrated in vacuo and the residue was taken up with methylene chloride. The mixture was then washed with water and conc. hydrochloric acid was added to the organic phase. The precipitate deposited was filtered off, washed with 2 N hydrochloric acid, dissolved in water and rendered alkaline with 20% strength NaOH. The residue was dried in vacuo.

WORKUP

后处理

  1. filtrationThe residue was filtered off
  2. concentrationthe solution was concentrated in vacuo
  3. washThe mixture was then washed with water and conc. hydrochloric acid
  4. additionwas added to the organic phase
  5. filtrationThe precipitate deposited was filtered off
  6. washwashed with 2 N hydrochloric acid
  7. dissolutiondissolved in water
  8. customThe residue was dried in vacuo