反応 #531800

反応方程式

coronene

succinic anhydride

aluminum chloride

→

yellow-green solid

収率 88.4%

γ-oxo-4-(coronen-1-yl)butanoic acid

収率 88.4%

溶媒

nitrobenzene

反応条件

後処理

1. 1
   その他The substance obtained here
2. 2
   その他was immersed in an ice bath
3. 3
   その他the 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
   温度The substance was cooled slowly down to room temperature
8. 8
   その他to precipitate a solid substance
9. 9
   ろ過The solid substance was collected by filtration
10. 10
    workup.ADDITIONThis solid substance was dispersed in 20 ml of xylene
11. 11
    温度was heated to 140° C
12. 12
    workup.DISSOLUTIONIn this manner, the solid substance was dissolved
13. 13
    温度The substance was then cooled slowly back to room temperature
14. 14
    その他to precipitate a solid substance
15. 15
    その他The solid substance obtained here
16. 16
    ろ過was collected by filtration
17. 17
    その他was dried under reduced pressure

実験手順

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.

出典