반응 #1463489

반응 방정식

1-chloroanthraquinone

1-ethylpropylamine

potassium acetate

→

1-(1-ethylpropylamino)anthraquinone

용매

water

반응 조건

후처리

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

실험 절차

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.

출처