반응 #531800

반응 방정식

coronene

succinic anhydride

aluminum chloride

→

yellow-green solid

수율 88.4%

γ-oxo-4-(coronen-1-yl)butanoic acid

수율 88.4%

용매

nitrobenzene

반응 조건

후처리

1. 1
   기타The substance obtained here
2. 2
   기타was immersed in an ice bath
3. 3
   기타the reaction container was removed from the ice bath
4. 4
   workup.ADDITION10 ml of cooled 2M hydrochloric acid was added
5. 5
   workup.WAITfollowed by 10-minute
6. 6
   workup.STIRRINGstirring
7. 7
   온도The substance was cooled slowly down to room temperature
8. 8
   기타to precipitate a solid substance
9. 9
   여과The solid substance was collected by filtration
10. 10
    workup.ADDITIONThis solid substance was dispersed in 20 ml of xylene
11. 11
    온도was heated to 140° C
12. 12
    workup.DISSOLUTIONIn this manner, the solid substance was dissolved
13. 13
    온도The substance was then cooled slowly back to room temperature
14. 14
    기타to precipitate a solid substance
15. 15
    기타The solid substance obtained here
16. 16
    여과was collected by filtration
17. 17
    기타was dried under reduced pressure

실험 절차

The coronene 81 (0.699 g, 2.33 mmol) and 0.514 g (5.14 mmol) of succinic anhydride were put into a 100-ml two-inlet flask, and a nitrogen substitution was performed. The substance obtained here was immersed in an ice bath. After 2.80 g (21.0 mmol) of aluminum chloride dispersed in 20 ml of nitrobenzene was slowly dripped onto the substance, the reaction container was removed from the ice bath, and the substance was stirred at room temperature for 5 hours. After the reaction was completed, 10 ml of cooled 2M hydrochloric acid was added, followed by 10-minute stirring. The substance was cooled slowly down to room temperature, to precipitate a solid substance. The solid substance was collected by filtration. This solid substance was dispersed in 20 ml of xylene, and was heated to 140° C. In this manner, the solid substance was dissolved. The substance was then cooled slowly back to room temperature, to precipitate a solid substance. The solid substance obtained here was collected by filtration, and was dried under reduced pressure, to obtain 0.825 g of the yellow-green solid substance 82.

출처