Methyl Isobutyl Ketone → HCID 86682208, Verbindung

HRID 2408220Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2408220
[F:1][C:2]([O:10][C:11]([F:20])([F:19])[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14])([C:6]([F:9])([F:8])[F:7])[C:3]([OH:5])=[O:4].[Cl-].[C:22]1([S+:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C(C(C)=O)C(C)C>ClCCl>[F:1][C:2]([O:10][C:11]([F:19])([F:20])[C:12]([F:18])([F:17])[C:13]([F:14])([F:15])[F:16])([C:6]([F:9])([F:8])[F:7])[C:3]([O-:5])=[O:4].[C:35]1([S+:28]([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=1

Komponenten

5

Edukt 3

HCID 7909Methyl Isobutyl KetoneHCID 61343Triphenylsulfonium chlorideHCID 114481Perfluoro-2-methyl-3-oxahexanoic acid

Produkt 1

HCID 86682208HCID 86682208, VerbindungAusbeute 35,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To 6.6 g (0.02 mol) of 2,3,3,3-tetrafluoro-2-(1,1,2,2,3,3,3-heptafluoropropoxy)propionic acid were added an amount (0.03 mol) of triphenylsulfonium chloride aqueous solution, 60 g of methyl isobutyl ketone, and 25 g of dichloromethane. An organic layer was taken out, and washed with 50 g of water three times. After the solvent was distilled off in vacuum, the residue was added to diisopropyl ether for crystallization. On filtration and drying, 4.2 g of white crystals was obtained (yield 35%). The compound thus obtained was analyzed by spectroscopy.

Aufarbeitung

  1. washwashed with 50 g of water three times
  2. distillationAfter the solvent was distilled off in vacuum
  3. additionthe residue was added to diisopropyl ether for crystallization
  4. filtrationOn filtration
  5. customdrying

Quellen und Nachweise

ORD-Eintrag
ord-7365501878884c4a9c5f5a2828aa7311
Quelldatensatz
uspto-grants-2014_08
Patentnummer
US08815492B2

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