HRID4674
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
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
- temperaturewas refluxed for 1 hour under azeotropic dehydration
- washThe mixture was washed with water (50 ml)
- dry with materiala saturated aqueous solution of sodium chloride (50 ml) successively, dried over magnesium sulfate
- customevaporated in vacuo
- customThe residual substance was recrystallized from ether