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Water → HCID 57736340, Verbindung

HRID 2261329
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2261329
F[C:2](F)([C:8]([F:14])([F:13])[C:9]([F:12])([F:11])[F:10])[CH:3]=[C:4](I)[CH2:5][OH:6].[OH2:16].Cl.[NH2:18]O.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[F:13][C:8]([F:14])([C:2]1[O:16][N:18]=[C:4]([CH2:5][OH:6])[CH:3]=1)[C:9]([F:12])([F:11])[F:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 6145864,4,5,5,6,6,6-Heptafluoro-2-iodohex-2-en-1-ol

Produkt 1

HCID 57736340HCID 57736340, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702Ethanol
Lösungsmittel

Versuchsvorschrift

8.9 g of 4,4,5,5,6,6,6-heptafluoro-2-iodo-2-hexene-1-ol was dissolved in 90 ml of ethanol, and 40 ml of water, 4.17 g of hydroxylamine hydrochloride and 20.70 g of potassium carbonate were then added. The mixture was stirred and heated under reflux for 20 hours. The reaction mixture was concentrated under reduced pressure. After water was added, the residue was extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 2.78 g of (5-pentafluoroethyl-isoxazol-3-yl)methanol.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 20 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionAfter water was added
  5. extractionthe residue was extracted with ethyl acetate
  6. washThe organic layer was washed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-27162c532c454ace84b871cc296cc441
Quelldatensatz
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07846956B2

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