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Sodium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonate → 4-Fluorophenyldiphenylsulfonium 1,1,3,3,3-pentafluoro-2-hydroxypropanesulfonate

HRID 1920614
ノート
印刷プレビュー

反応式

HRID 1920614 の反応式
[Cl-].[F:2][C:3]1[CH:8]=[CH:7][C:6]([S+:9]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:5][CH:4]=1.[F:22][C:23]([F:34])([S:30]([O-:33])(=[O:32])=[O:31])[CH:24]([OH:29])[C:25]([F:28])([F:27])[F:26].[Na+]>>[F:34][C:23]([F:22])([S:30]([O-:33])(=[O:31])=[O:32])[CH:24]([OH:29])[C:25]([F:26])([F:28])[F:27].[F:2][C:3]1[CH:8]=[CH:7][C:6]([S+:9]([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 86612200Sodium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonateHCID 866496604-Fluorophenyldiphenylsulfonium chloride

生成物 1

HCID 866496594-Fluorophenyldiphenylsulfonium 1,1,3,3,3-pentafluoro-2-hydroxypropanesulfonate収率 70%

実験手順

An amount (0.2 mole) of the 4-fluorophenyldiphenyl-sulfonium chloride aqueous solution in Synthesis Example 1 was combined with an amount (0.2 mole) of the sodium 1,1,3,3,3-pentafluoro-2-hydroxypropanesulfonate aqueous solution in Synthesis Example 2, followed by twice extraction with 500 g of dichloromethane. Through the steps of washing the organic layer with water, distilling off the solvent in vacuum, adding isopropyl ether for crystallization, filtration and drying, the target compound was obtained. White crystals, 71.5 g, yield 70% (based on diphenyl sulfoxide).

後処理

  1. extractionfollowed by twice extraction with 500 g of dichloromethane
  2. washThrough the steps of washing the organic layer with water
  3. distillationdistilling off the solvent in vacuum
  4. additionadding isopropyl ether
  5. customfor crystallization, filtration
  6. customdrying
  7. customthe target compound was obtained

出典と根拠

ORDレコード
ord-46ec399a4dcf4a5e83a24652a9d09317
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08173354B2

反応ノート

読み込み中…

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