반응 #52253

반응 방정식

2,2-bis[N-(2-nitrophenyl)-(3-aminophenyl)]hexafluoropropane

hydrogen

→

2,2-bis[N-(2-aminophenyl)-(3-aminophenyl)]hexafluoropropane

수율 94.9%

용매

ethyl acetate

반응 조건

후처리

1. 1
   기타After that, reaction
2. 2
   기타was conducted at room temperature under a hydrogen
3. 3
   기타for 18 hours
4. 4
   기타The obtained reaction solution
5. 5
   여과was filtered with cerite
6. 6
   기타to remove the catalyst, and ethyl acetate
7. 7
   기타was removed under reduced pressure
8. 8
   기타The residue was recrystallized

실험 절차

20 g (34.7 mmol) of 2,2-bis[N-(2-nitrophenyl)-(3-aminophenyl)]hexafluoropropane synthesized above were dissolved in 200 ml of ethyl acetate. Thereto was added 1 g of 10% palladium carbon as a catalyst, and replacement with hydrogen was carried out. After that, reaction was conducted at room temperature under a hydrogen pressure of 1.01 MPa (10 atm) for 18 hours with stirring vigorously. The obtained reaction solution was filtered with cerite to remove the catalyst, and ethyl acetate was removed under reduced pressure. The residue was recrystallized by using a chloroform-hexane mixed solution, and ethanol-water mixed solution to obtain 17 g of 2,2-bis[N-(2-aminophenyl)-(3-aminophenyl)]hexafluoropropane (hereinafter mNPN-AF) in white solid(yeild: 95%).

출처