Reaktion #1463489

Reaktionsgleichung

1-chloroanthraquinone

1-ethylpropylamine

potassium acetate

→

1-(1-ethylpropylamino)anthraquinone

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reaction vessel was sealed
2. 2
   Temperaturmaintained at that temperature for 12 hours
3. 3
   SonstigeThe oil bath was removed
4. 4
   ExtraktionThe solid was extracted with methylene chloride
5. 5
   Sonstigethe insoluble materials removed by filtration
6. 6
   SonstigeThe solvent was removed
7. 7
   Sonstigethe solid recrystallized from hot methanol
8. 8
   SonstigeThe material was chromatographed on a silica gel column

Vorschrift

A Parr stainless steel high pressure reactor was charged with 1-chloroanthraquinone (24.3 g), 1-ethylpropylamine (17.5 g), potassium acetate.(14.0 g), activated copper metal (0.7 g), and water (0.05 g). The reaction vessel was sealed and heated to a temperature of 180° C. in an oil bath and maintained at that temperature for 12 hours. The oil bath was removed and the vessel was allowed to return to ambient conditions. The solid was extracted with methylene chloride and the insoluble materials removed by filtration. The solvent was removed and the solid recrystallized from hot methanol. The material was chromatographed on a silica gel column using toluene as the eluent.

Quelle