반응 #992720

반응 방정식

2,7-bis(acetylamino)thianthrene

hydrochloric acid

→

2,7-diaminothianthrene

수율 91.0%

용매

ethanol

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도under reflux for 6 hours
3. 3
   여과a precipitate was collected by filtration
4. 4
   workup.ADDITIONThe precipitate was added to a mixture of 13.5 ml of concentrated hydrochloric acid and 355 ml of water
5. 5
   기타the insoluble matters were separated by filtration
6. 6
   workup.ADDITIONThe filtered mother liquor was poured into an aqueous solution of sodium hydroxide
7. 7
   여과the precipitate or 2,7-diaminothianthrene was collected by filtration

실험 절차

A mixture of 5.75 g (0.0174 mole) of 2,7-bis(acetylamino)thianthrene, 12 ml of concentrated hydrochloric acid, and 140 ml of ethanol was heated under reflux for 6 hours. The reaction mixture was cooled to room temperature and a precipitate was collected by filtration. The precipitate was added to a mixture of 13.5 ml of concentrated hydrochloric acid and 355 ml of water and the insoluble matters were separated by filtration. The filtered mother liquor was poured into an aqueous solution of sodium hydroxide and the precipitate or 2,7-diaminothianthrene was collected by filtration. The yield was 3.7 g (0.0158 mole, 91% yield) and the purity was 88.2 area % (HPLC, 254 nm).

출처