反応 #531798

反応方程式

perylene

succinic anhydride

aluminum chloride

→

brownish solid

収率 100.2%

γ-oxo-4-(perylen-1-yl)butanoic acid

収率 100.2%

溶媒

methylene chloride

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.ADDITION40 ml of cooled 2M hydrochloric acid was added
5. 5
   workup.WAITfollowed by 30-minute
6. 6
   workup.STIRRINGstirring
7. 7
   その他The solid substance obtained here
8. 8
   ろ過was collected by filtration
9. 9
   workup.ADDITIONThis solid substance was dispersed in 100 ml of xylene
10. 10
    温度was heated to 140° C.
11. 11
    抽出to extract the impurities
12. 12
    温度After the substance was cooled slowly back to room temperature
13. 13
    ろ過the solid substance was collected by filtration
14. 14
    その他was dried under reduced pressure

実験手順

The perylene 71 (5.01 g, 19.8 mmol) and 4.34 g (43.4 mmol) of succinic anhydride were put into a 500-ml three-inlet flask, and a nitrogen substitution was performed. The substance obtained here was immersed in an ice bath. After 16.3 g (122 mmol) of aluminum chloride dispersed in 200 ml of methylene chloride was slowly dripped onto the substance, the reaction container was removed from the ice bath, and the substance was stirred at room temperature for 13 hours. After the reaction was completed, 40 ml of cooled 2M hydrochloric acid was added, followed by 30-minute stirring. The solid substance obtained here was collected by filtration. This solid substance was dispersed in 100 ml of xylene, and was heated to 140° C., to extract the impurities. After the substance was cooled slowly back to room temperature, the solid substance was collected by filtration, and was dried under reduced pressure, to obtain 6.99 g of the brownish solid substance 72.

出典