Benzene → Pentafluoroethylphenyliodonium trifluoromethanesulfonate

HRID 2285860ノート

反応式

HRID 2285860 の反応式
FC(F)(F)C(O[I:6](OC(=O)C(F)(F)F)[C:7]([F:13])([F:12])[C:8]([F:11])([F:10])[F:9])=O.FC(F)(F)C(O)=O.[F:30][C:31]([F:37])([F:36])[S:32]([OH:35])(=[O:34])=[O:33].[CH:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1>>[F:30][C:31]([F:37])([F:36])[S:32]([O-:35])(=[O:34])=[O:33].[F:13][C:7]([I+:6][C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)([F:12])[C:8]([F:9])([F:10])[F:11]

参加物

5

反応物 4

HCID 241BenzeneHCID 6422Trifluoroacetic acidHCID 62406Trifluoromethanesulfonic acidHCID 12918315Di(trifluoroacetoxy)iodopentafluoroethane

生成物 1

HCID 11488264Pentafluoroethylphenyliodonium trifluoromethanesulfonate収率 55%

実験手順

To a mixture of 6.05 g of di(trifluoroacetoxy)iodopentafluoroethane and 45 ml of trifluoroacetic acid was added 1.1 ml of trifluoromethanesulfonic acid while cooling in an ice bath and stirring, and thereafter 1.2 ml of benzene was added dropwise to the mixture. After completion of the addition, the mixture was stirred for 4.5 hours and the solvent was distilled off to obtain a crystalline solid which was then recrystallized from chloroform to obtain 3.32 g (55% yield) of pentafluoroethylphenyliodonium trifluoromethanesulfonate as colorless flake crystals.

後処理

  1. temperaturewhile cooling in an ice bath
  2. additionAfter completion of the addition
  3. stirringthe mixture was stirred for 4.5 hours
  4. distillationthe solvent was distilled off
  5. customto obtain a crystalline solid which
  6. customwas then recrystallized from chloroform

出典と根拠

ORDレコード
ord-3f9afabd44104bcfa85d938c58b60f01
出典データセット
uspto-grants-1982_04
特許番号
US04324741

反応ノート

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