반응 #1973930

반응 방정식

N-(2-hydroxy-1-p-tolyl-propyl)-3-methylbezamide

phosphorus (V) oxide

decahydronaphtalene

→

1-(3-methylphenyl)-4,7-dimethylisoquinoline

반응 조건

후처리

1. 1
   기타After completion of the reaction
2. 2
   추출the reaction mixture was extracted with dichloromethane and water
3. 3
   workup.DISTILLATIONdistilled under reduced pressure
4. 4
   기타The resulting residue was purified by silica gel column chromatography
5. 5
   workup.DISTILLATIONThe eluate was distilled under reduced pressure
6. 6
   기타The residue was recrystallized from dichloromethane and petroleum ether
7. 7
   여과filtered

실험 절차

N-(2-hydroxy-1-p-tolyl-propyl)-3-methylbezamide (2.1 mmol), phosphorus (V) oxide (10 mmol) and decahydronaphtalene (50 mmol) were put in a dried two-neck round-bottom flask. Then, the mixture was stirred at 120 for 5 hours. After completion of the reaction, the reaction mixture was extracted with dichloromethane and water and distilled under reduced pressure. The resulting residue was purified by silica gel column chromatography. The eluate was distilled under reduced pressure. The residue was recrystallized from dichloromethane and petroleum ether, and filtered to yield 1-(3-methylphenyl)-4,7-dimethylisoquinoline.

출처