تفاعل #1884945

ord-0fbc5c7f57904aa7b5dc0e5c6e36a6ea

معادلة التفاعل

O=C(O)C(F)(F)F
Trifluoroacetic acid
NNC(=O)C(F)(F)F
trifluoroacethydrazide
O=C(NNC(=O)C(F)(F)F)C(F)(F)F
1,2-bis(trifluoroacetyl)hydrazine

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

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

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08343260B2uspto-grants-2013_01