تفاعل #1106607

معادلة التفاعل

Trifluoroacetic acid

trifluoroacethydrazide

→

1,2-bis(trifluoroacetyl)hydrazine

المذيبات

benzene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was heated
2. 2
   درجة الحرارةunder reflux for 2 h
3. 3
   أخرىA Dean and Stark trap was fitted
4. 4
   درجة الحرارةreflux
5. 5
   درجة الحرارةReflux
6. 6
   أخرىwas continued in the absence of the Dean and Stark trap (3 h)
7. 7
   أخرى(20 h)
8. 8
   ترشيحThe resulting white solid was collected by filtration
9. 9
   أخرىdried in vacuum

الإجراء التجريبي

Trifluoroacetic acid (7.6 mL, 0.1 mol) was added to a stirred solution of trifluoroacethydrazide (12.8 g, 0.1 mol) in benzene (100 mL) and the mixture was heated under reflux for 2 h. A Dean and Stark trap was fitted, and reflux was continued for 3 h. Reflux was continued in the absence of the Dean and Stark trap (3 h) and then with the trap refitted (20 h). The resulting white solid was collected by filtration, dried in vacuum and identified as 1,2-bis(trifluoroacetyl)hydrazine (16.5 g, 73%). M.p. 173-175° C.

المصدر