Sodium Iodide → N-(2,2,3,3,4,4,4-heptafluorobutyl)-5-iodo-N-methylpentanesulfonamide

HRID 742953Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 742953
[I-:1].[Na+].Cl[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][S:9]([N:12]([CH2:14][C:15]([F:24])([F:23])[C:16]([F:22])([F:21])[C:17]([F:20])([F:19])[F:18])[CH3:13])(=[O:11])=[O:10]>C(C(C)=O)C>[F:23][C:15]([F:24])([C:16]([F:22])([F:21])[C:17]([F:20])([F:19])[F:18])[CH2:14][N:12]([CH3:13])[S:9]([CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][I:1])(=[O:11])=[O:10]

Komponenten

4

Edukt 2

HCID 5238Sodium IodideHCID 197110325-chloro-N-(2,2,3,3,4,4,4-heptafluorobutyl)-N-methyl-pentanesulfonamide

Produkt 1

HCID 19711036N-(2,2,3,3,4,4,4-heptafluorobutyl)-5-iodo-N-methylpentanesulfonamideAusbeute 96,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6569Methyl Ethyl KetoneLösungsmittel

Versuchsvorschrift

300 mg of sodium iodide were added to a solution of 355 mg of the product of Step A in 3 ml of methyl ethyl ketone and the mixture was refluxed for 4 hours. After evaporation of the solvent, the residue was taken up in water and extracted with ethyl acetate. The extracts were washed with an aqueous solution of sodium thiosulfate, then of sodium chloride, and evaporated to dryness under reduced pressure to obtain 425 mg of the expected product in the form of a colourless oil which slowly crystallized.

Aufarbeitung

  1. temperaturethe mixture was refluxed for 4 hours
  2. customAfter evaporation of the solvent
  3. extractionextracted with ethyl acetate
  4. washThe extracts were washed with an aqueous solution of sodium thiosulfate
  5. customof sodium chloride, and evaporated to dryness under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-4b22165e5e3a483394309476474b57c8
Quelldatensatz
uspto-grants-1996_09
Patentnummer
US05556845

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