반응 #992717

반응 방정식

acetic anhydride

2,7-diaminodibenzodioxin

pyridine

toluene

THF

→

2,7-bis(acetylamino)dibenzodioxin

수율 82.0%

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the dropwise addition
2. 2
   workup.STIRRINGthe mixture was stirred overnight
3. 3
   여과a precipitate was recovered by filtration
4. 4
   기타dried under reduced pressure

실험 절차

To a mixture of 900 ml of toluene and 900 ml of THF were added 50.0 g (0.233 mole) of 2,7-diaminodibenzodioxin and 55.3 g (0.699 mole) of pyridine and to the resulting mixture was added 59.5 g (0.583 mole) of acetic anhydride in drops over a period of 10 minutes at room temperature with stirring. After the dropwise addition, the mixture was stirred overnight and a precipitate was recovered by filtration. The precipitate was reslurried with toluene (250 mix 2) and dried under reduced pressure to give 57.0 g (0.191 mole, 82.0% yield) of 2,7-bis(acetylamino)dibenzodioxin. The product showed a purity of 99.3 area % (HPLC, 254 nm).

출처