Iodopentafluoroethane → HCID 178506327, Verbindung

HRID 2243281

Reaktionsgleichung

Reaktionsgleichung von HRID 2243281
I[C:2]1[C:3]([C:7]([F:13])([F:12])[C:8]([F:11])([F:10])[F:9])=[N:4][NH:5][CH:6]=1.I[C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17]>[Cu].CN(C=O)C>[F:12][C:7]([F:13])([C:3]1[C:2]([C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17])=[CH:6][NH:5][N:4]=1)[C:8]([F:11])([F:10])[F:9]

Komponenten

5

Edukt 2

HCID 9636IodopentafluoroethaneHCID 178506332HCID 178506332, Verbindung

Produkt 1

HCID 178506327HCID 178506327, VerbindungAusbeute 9,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23978CopperKatalysatorHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
122.5 °C

Versuchsvorschrift

4-Iodo-3-pentafluoroethyl-1H-pyrazole (12.48 g), copper powder (7.63 g), iodopentafluoroethane (29.50 g) and DMF (60 ml) were set in an autoclave and heated and stirred for 8 hours, maintaining the inside temperature of 120-125° C. After cooling to room temperature, the insoluble material was filtered off through Celite and washed with diethyl ether. The filtrate was diluted with water and extracted with diethyl ether. The organic phase was washed with water and dried over sodium sulfate, and concentrated under the reduced pressure. The crude product was distilled under reduced pressure to obtain 3,4-bis-pentafluoroethyl-1H-pyrazole (1.20 g), bp. 110-115° C./20 mbar.

Aufarbeitung

  1. temperatureheated
  2. temperatureAfter cooling to room temperature
  3. filtrationthe insoluble material was filtered off through Celite
  4. washwashed with diethyl ether
  5. additionThe filtrate was diluted with water
  6. extractionextracted with diethyl ether
  7. washThe organic phase was washed with water
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated under the reduced pressure
  10. distillationThe crude product was distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-e303a7e8bf0b4a68b5db9d22217ccab1
Quelldatensatz
uspto-grants-2010_03
Patentnummer
US07674807B2

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