反応 #1973930

反応方程式

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

phosphorus (V) oxide

decahydronaphtalene

→

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

反応条件

後処理

1. 1
   その他After completion of the reaction
2. 2
   抽出the reaction mixture was extracted with dichloromethane and water
3. 3
   workup.DISTILLATIONdistilled under reduced pressure
4. 4
   その他The resulting residue was purified by silica gel column chromatography
5. 5
   workup.DISTILLATIONThe eluate was distilled under reduced pressure
6. 6
   その他The residue was recrystallized from dichloromethane and petroleum ether
7. 7
   ろ過filtered

実験手順

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.

出典