반응 #992716

반응 방정식

anisole

2,7-dinitrodibenzodioxin

hydrogen

→

2,7-diaminodibenzodioxin

수율 46.1%

용매

THF

반응 조건

후처리

1. 1
   기타The 10% palladium/carbon was removed by filtration
2. 2
   workup.ADDITIONa precipitate containing the 10% palladium/carbon
3. 3
   여과was collected by filtration
4. 4
   세척the precipitate was rinsed with THF
5. 5
   농축The rinsings were concentrated
6. 6
   기타dried under reduced pressure

실험 절차

To a mixture of 1200 ml of anisole and 800 ml of THF were added 69.7 g (0.254 mole) of 2,7-dinitrodibenzodioxin and 22.2 g of 10% palladium/carbon and hydrogen gas was passed through the mixture with stirring at room temperature for 8 hours. The 10% palladium/carbon was removed by filtration, then a precipitate containing the 10% palladium/carbon was collected by filtration, and the precipitate was rinsed with THF. The rinsings were concentrated and dried under reduced pressure to give 25.0 g (0.117 mole, 46.0% yield) of 2,7-diaminodibenzodioxin. The product showed a purity of 98.1% (HPLC, 254 nm).

출처