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

HRID 1019425ノート

反応式

HRID 1019425 の反応式
[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]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 229753Trifluoroacetohydrazide

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dc8fa5cbd166445cb6dbc2f280a80cfe
出典データセット
uspto-grants-2014_05
特許番号
US08715395B2

反応ノート

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