Reaktion #4770

Reaktionsgleichung

diethyl ether

3-nitrobenzaldehyde

acetylacetone

acetic acid

→

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

Ausbeute 53.5%

Lösungsmittel

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed for 1 hour under azeotropic dehydration
2. 2
   WaschenThe mixture was washed with water (50 ml)
3. 3
   Trocknena saturated aqueous solution of sodium chloride (50 ml) successively, dried over magnesium sulfate
4. 4
   Sonstigeevaporated in vacuo
5. 5
   SonstigeThe residual substance was recrystallized from ether

Vorschrift

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).

Quelle