تفاعل #992720

معادلة التفاعل

2,7-bis(acetylamino)thianthrene

hydrochloric acid

→

2,7-diaminothianthrene

المردود 91.0%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةunder reflux for 6 hours
3. 3
   ترشيحa 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
   أخرىthe insoluble matters were separated by filtration
6. 6
   workup.ADDITIONThe filtered mother liquor was poured into an aqueous solution of sodium hydroxide
7. 7
   ترشيحthe precipitate or 2,7-diaminothianthrene was collected by filtration

الإجراء التجريبي

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).

المصدر