反应 #1973930

反应方程式

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

phosphorus (V) oxide

decahydronaphtalene

→

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

反应条件

后处理

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

实验过程

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.

来源