反应详情

15.0 g of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane and 50.0 cc of methanol were put into a 100-cc four-neck flask equipped with a thermometer, a Dimroth condenser and a stirrer, and stirred therein, to which was added 0.23 g (dry weight) of E196R/W5%Pd (trade name, 5% palladium-carbon catalyst, manufactured by Degussa Japan Co.). This was heated and kept at 60 to 65° C., to which was dropwise added 11.8 g of an aqueous solution of 60% hydrazine monohydrate over a period of 20 minutes. If desired, the reaction system was cooled, as generating heat during the reaction. After the aqueous hydrazine solution was added, the mixture was stirred at 70° C. for 30 minutes, and then gradually cooled to room temperature. After the catalyst was removed through filtration, methanol and water were evaporated out of the reaction mixture to obtain a crude product of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane. The crude yield was 12.6 g (98%). The purity in liquid chromatography was 98.3% (area %).

1. customequipped with a thermometer
2. additionto which was added
3. dry with material0.23 g (dry weight) of E196R/W5%Pd (trade name, 5% palladium-carbon catalyst, manufactured by Degussa Japan Co.)
4. temperatureThis was heated
5. customkept at 60 to 65° C., to which
6. customof 20 minutes
7. temperaturethe reaction system was cooled
8. temperatureas generating heat during the reaction
9. additionAfter the aqueous hydrazine solution was added
10. stirringthe mixture was stirred at 70° C. for 30 minutes
11. customAfter the catalyst was removed through filtration, methanol and water
12. customwere evaporated out of the reaction mixture