Water → HCID 22061606, Verbindung

HRID 2104307Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2104307
[N-:1]=[N+:2]=[N-:3].[Na+].O.[F:6][C:7]([F:35])([CH2:30][CH2:31][C:32](Cl)=[O:33])[C:8]([F:29])([F:28])[C:9]([F:27])([F:26])[C:10]([F:25])([F:24])[C:11]([F:23])([F:22])[C:12]([F:21])([F:20])[C:13]([F:19])([F:18])[C:14]([F:17])([F:16])[F:15].COC>CC(C)=O>[F:6][C:7]([F:35])([CH2:30][CH2:31][C:32]([N:1]=[N+:2]=[N-:3])=[O:33])[C:8]([F:28])([F:29])[C:9]([F:26])([F:27])[C:10]([F:25])([F:24])[C:11]([F:22])([F:23])[C:12]([F:21])([F:20])[C:13]([F:19])([F:18])[C:14]([F:17])([F:16])[F:15]

Komponenten

6

Edukt 4

HCID 962Water2×HCID 8254Dimethyl EtherHCID 33557Sodium Azide2×HCID 108641354,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,11-Heptadecafluoroundecanoyl chloride

Produkt 1

HCID 22061606HCID 22061606, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

Sodium azide (6.0 g) was put in a 250 mL round-bottom flask (2-neck) equipped with a thermometer. H2O (20 mL) was added to dissolve sodium azide. It was cooled on an ice-water bath. A solution of 3-(perfluorooctyl)propionyl chloride (12.9 g) in acetone (25 mL) was added dropwise to keep the temperature below 12° C. The mixture was vigorously stirred for 2 h. Dimethyl ether (100 mL) and water (100 mL) are added, and the mixture was vigorously stirred for 1 min. After the separation of two layers, the aqueous layer was extracted with ether (2×50 mL). The ether layers were combined, and are washed with water (3×100 mL) and brine. After drying over MgSO4, the solvent was removed under vacuum to give a mixture of white solid and liquid (12.0 g) that was immediately used for the next reaction.

Aufarbeitung

  1. custom(2-neck) equipped with a thermometer
  2. temperatureIt was cooled on an ice-water bath
  3. customthe temperature below 12° C
  4. stirringthe mixture was vigorously stirred for 1 min
  5. customAfter the separation of two layers
  6. extractionthe aqueous layer was extracted with ether (2×50 mL)
  7. washare washed with water (3×100 mL) and brine
  8. dry with materialAfter drying over MgSO4
  9. customthe solvent was removed under vacuum
  10. customto give
  11. customwas immediately used for the next reaction

Quellen und Nachweise

ORD-Eintrag
ord-c57d6cdc6c22450c8d9c0fc5112622f0
Quelldatensatz
uspto-grants-2009_08
Patentnummer
US07576245B2

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