HRID1729763

反应详情

EQUATION

反应方程式

HRID 1729763 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 2-(1-allyloxyaminopropylidene)-5,5-dimethylcyclohexane-1,3-dione (2.5 g) in acetone (30 ml), sodium hydroxide (0.4 g) in water (2 ml) was added at room temperature and then benzyl bromide (2.0 g) was added. After stirring for 10 hours at 60° C the reaction mixture was poured into ice-water and extracted with chloroform. The extract was washed with one normal sodium hydroxide and dried over magnesium sulfate. The solvent was removed in vacuo and an oily substance which solidified on standing at 0° C was obtained. Recrystallization from the mixture of methanol and water gave the desired product as crystal.

WORKUP

后处理

  1. extractionextracted with chloroform
  2. washThe extract was washed with one normal sodium hydroxide
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed in vacuo
  5. customon standing at 0° C
  6. customwas obtained
  7. customRecrystallization
  8. additionfrom the mixture of methanol and water