Thiophenol → HCID 19821224、化合物

HRID 1030204ノート

反応式

HRID 1030204 の反応式
F[C:2]1[CH:33]=[CH:32][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([O:14][C:15]([O:23][C:24]3[CH:29]=[CH:28][CH:27]=[C:26]([O:30][CH3:31])[CH:25]=3)([F:22])[CH:16]([F:21])[C:17]([F:20])([F:19])[F:18])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[C:40]1([SH:46])[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1>CN(C)C=O>[C:40]1([S:46][C:2]2[CH:3]=[CH:4][C:5]([C:6]([C:8]3[CH:13]=[CH:12][C:11]([O:14][C:15]([O:23][C:24]4[CH:29]=[CH:28][CH:27]=[C:26]([O:30][CH3:31])[CH:25]=4)([F:22])[CH:16]([F:21])[C:17]([F:19])([F:20])[F:18])=[CH:10][CH:9]=3)=[O:7])=[CH:32][CH:33]=2)[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1

参加物

5

反応物 3

HCID 7969ThiophenolHCID 11430Potassium CarbonateHCID 19821204HCID 19821204、化合物

生成物 1

HCID 19821224HCID 19821224、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

33 g 4-fluoro-4'-(1-(3-methoxyphenoxy)-1,2,3,3,3-pentafluoro-propoxy)benzophenone, 10 g potassium carbonate, 7.7 g thiophenol, and 100 ml dimethylformamide were stirred together for eight hours at 100° C., then allowed to cool to room temperature. After cooling, the solids were removed from the mixture by filtration, and the low boilers were removed by distillation at 200° C./0.5 mm Hg. The resulting product was distilled at 240°-300° C./0.5 mm Hg. NMR spectra and gas chromatography confirmed that the desired benzophenone was prepared.

後処理

  1. temperatureAfter cooling
  2. customthe solids were removed from the mixture by filtration
  3. customthe low boilers were removed by distillation at 200° C./0.5 mm Hg
  4. distillationThe resulting product was distilled at 240°-300° C./0.5 mm Hg
  5. customwas prepared

出典と根拠

ORDレコード
ord-5c7f59391f394b18943bc6c57db533ea
出典データセット
uspto-grants-1992_04
特許番号
US05104559

反応ノート

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