反応 #4770

反応方程式

diethyl ether

3-nitrobenzaldehyde

acetylacetone

acetic acid

→

1-acetyl-1-(3-nitrobenzyliden)acetone

収率 53.5%

溶媒

benzene

反応条件

後処理

1. 1
   温度was refluxed for 1 hour under azeotropic dehydration
2. 2
   洗浄The mixture was washed with water (50 ml)
3. 3
   乾燥a saturated aqueous solution of sodium chloride (50 ml) successively, dried over magnesium sulfate
4. 4
   その他evaporated in vacuo
5. 5
   その他The residual substance was recrystallized from ether

実験手順

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).

出典