反应 #531800

反应方程式

coronene

succinic anhydride

aluminum chloride

→

yellow-green solid

收率 88.4%

γ-oxo-4-(coronen-1-yl)butanoic acid

收率 88.4%

溶剂

nitrobenzene

反应条件

后处理

1. 1
   其他The substance obtained here
2. 2
   其他was immersed in an ice bath
3. 3
   其他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
   其他to precipitate a solid substance
9. 9
   过滤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
    其他to precipitate a solid substance
15. 15
    其他The solid substance obtained here
16. 16
    过滤was collected by filtration
17. 17
    其他was dried under reduced pressure

实验过程

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.

来源