Trifluoroacetic acid → 2,2,2-Trifluoro-N'-(trifluoroacetyl)acetohydrazide

HRID 1019425노트

반응식

HRID 1019425 반응식
[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=O.[F:8][C:9]([F:15])([F:14])[C:10]([NH:12][NH2:13])=[O:11]>C1C=CC=CC=1>[F:8][C:9]([F:15])([F:14])[C:10]([NH:12][NH:13][C:3](=[O:5])[C:2]([F:7])([F:6])[F:1])=[O:11]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 229753Trifluoroacetohydrazide

생성물 1

HCID 2297542,2,2-Trifluoro-N'-(trifluoroacetyl)acetohydrazide

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 h
  3. customA Dean and Stark trap was fitted
  4. temperaturereflux
  5. temperatureReflux
  6. customwas continued in the absence of the Dean and Stark trap (3 h)
  7. custom(20 h)
  8. filtrationThe resulting white solid was collected by filtration
  9. customdried in vacuum

출처 및 근거

ORD 기록
ord-dc8fa5cbd166445cb6dbc2f280a80cfe
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08715395B2

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