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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
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HRID 1920614 반응식
[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
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참가 물질

3

반응물 2

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

생성물 1

HCID 866496594-Fluorophenyldiphenylsulfonium 1,1,3,3,3-pentafluoro-2-hydroxypropanesulfonate수율 70%

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-46ec399a4dcf4a5e83a24652a9d09317
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08173354B2

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