Reaktion #1723996

Reaktionsgleichung

4-formyl-1-tritylimidazole

2,2'-(5-bromomethyl-1,3-phenylene)di(2-methylpropiononitrile)

acetonitrile

acetic acid

→

2,2'-[5-(5-formylimidazol-1-yl)-1,3-phenylene]di(2-methylpropiononitrile)

Lösungsmittel

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturunder reflux for 30 h
3. 3
   Temperaturthe mixture was then heated at 90° for 1 h
4. 4
   Waschenwashed with ether
5. 5
   Extraktionthe mixture was extracted three times with ethyl acetate
6. 6
   SonstigeThe combined extracts were dried
7. 7
   Sonstigeevaporated to dryness
8. 8
   Sonstigethe residue was purified by flash chromatography

Vorschrift

A mixture of 4-formyl-1-tritylimidazole (0.5 g), 2,2'-(5-bromomethyl-1,3-phenylene)di(2-methylpropiononitrile) and acetonitrile (2 ml) was heated under reflux for 30 h. The reaction mixture was treated with acetic acid (8 ml) and water (2 ml) and the mixture was then heated at 90° for 1 h. The mixture was diluted with water (20 ml) and washed with ether, the aqueous phase was basified with sodium carbonate, and the mixture was extracted three times with ethyl acetate. The combined extracts were dried and evaporated to dryness, and the residue was purified by flash chromatography using methanol (2% by volume) in chloroform as eluant, to give 2,2'-[5-(5-formylimidazol-1-yl)-1,3-phenylene]di(2-methylpropiononitrile), mp 108°-111°.

Quelle