HRID4674

反应详情

EQUATION

反应方程式

HRID 4674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3-nitrobenzaldehyde (20 g), acetylacetone (13.25 g), acetic acid (1.58 g), and piperidine (0.45 g) in benzene (20 ml) was refluxed for 1 hour under azeotropic dehydration. To the reaction mixture was added diethyl ether (100 ml). The mixture was washed with water (50 ml) and a saturated aqueous solution of sodium chloride (50 ml) successively, dried over magnesium sulfate, and evaporated in vacuo. The residual substance was recrystallized from ether to afford 1-acetyl-1-(3-nitrobenzyliden)acetone(16.5 g).

WORKUP

后处理

  1. temperaturewas refluxed for 1 hour under azeotropic dehydration
  2. washThe mixture was washed with water (50 ml)
  3. dry with materiala saturated aqueous solution of sodium chloride (50 ml) successively, dried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residual substance was recrystallized from ether