反応 #531799

反応方程式

compound 72

γ-oxo-4-(perylen-1-yl)butanoic acid

hydrazine

sodium hydroxide

→

black solid

収率 99.8%

4-(perylen-1-yl)butanoic acid

収率 99.8%

溶媒

diethylene glycol

反応条件

後処理

1. 1
   workup.WAITfollowed by 90-minute
2. 2
   温度refluxing in a 180-° C
3. 3
   workup.DISTILLATIONThe excess hydrazine and water were distilled away
4. 4
   その他to precipitate a solid substance
5. 5
   ろ過The solid substance was collected by filtration
6. 6
   洗浄was washed with ion-exchange water and 2M hydrochloric acid
7. 7
   その他by drying under reduced pressure
8. 8
   workup.ADDITIONThis solid substance was dispersed in 10 ml of xylene
9. 9
   温度was heated to 140° C
10. 10
    workup.DISSOLUTIONIn this manner, the solid substance was dissolved
11. 11
    温度After that, the substance was cooled slowly back to room temperature
12. 12
    その他to precipitate a solid substance
13. 13
    ろ過The solid substance generated here was collected by filtration
14. 14
    その他was dried under reduced pressure

実験手順

The compound 72 (0.390 g, 1.11 mmol), 0.4 ml of 79% aqueous hydrazine, and 0.290 g (7.25 mmol) of sodium hydroxide were dissolved in 3.0 ml of diethylene glycol, followed by 90-minute refluxing in a 180-° C. oil bath. The excess hydrazine and water were distilled away, and the refluxing was continued for two more hours. After the reaction was completed, the solution was cooled back to room temperature, to precipitate a solid substance. The solid substance was collected by filtration, and was washed with ion-exchange water and 2M hydrochloric acid, followed by drying under reduced pressure. This solid substance was dispersed in 10 ml of xylene, and was heated to 140° C. In this manner, the solid substance was dissolved. After that, the substance was cooled slowly back to room temperature, to precipitate a solid substance. The solid substance generated here was collected by filtration, and was dried under reduced pressure, to obtain 0.375 g of the black solid substance 73.

出典