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2,2,3,3,3-Pentafluoropropanol → Methyl 2,2,3,3,3-pentafluoropropyl carbonate

HRID 1781230
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1781230
[F:1][C:2]([F:9])([C:5]([F:8])([F:7])[F:6])[CH2:3][OH:4].[C:10](=O)([O:13]C)[O:11][CH3:12]>C[O-].[Na+].CO>[C:10](=[O:13])([O:4][CH2:3][C:2]([F:9])([F:1])[C:5]([F:8])([F:7])[F:6])[O:11][CH3:12]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 98722,2,3,3,3-PentafluoropropanolHCID 12021Dimethyl Carbonate

Produkt 1

HCID 18183634Methyl 2,2,3,3,3-pentafluoropropyl carbonateAusbeute 51 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 23694274Sodium methanolate methanolKatalysator

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

In a flask (500-ml volume) equipped with 10 distillation columns, 2,2,3,3,3-pentafluoropropanol (100 g, 0.67 mol), dimethyl carbonate (180 g, 2.0 mol) and a 28% sodium methoxide/methanol solution (1.3 g) were charged. The flask was heated to 120° C. to allow the starting materials to react for 10 hours while removing the methanol from the distillation columns by evaporation. After allowing the mixture to cool to room temperature, an aqueous solution of ammonium chloride was added to the mixture and the mixture was shaken to remove the sodium methoxide. The organic layer was washed with water, dried and distilled to give methyl 2,2,3,3,3-pentafluoropropyl carbonate as a colorless liquid (71 g, yield 51%). The chemical structure of the produced compound was determined based on the IR and NMR absorbance spectra shown in FIG. 7 and FIG. 8 respectively and the mass spectrometry spectrum (M/e=208).

Aufarbeitung

  1. customto react for 10 hours
  2. customwhile removing the methanol
  3. distillationfrom the distillation columns
  4. customby evaporation
  5. temperatureto cool to room temperature
  6. additionan aqueous solution of ammonium chloride was added to the mixture
  7. customto remove the sodium methoxide
  8. washThe organic layer was washed with water
  9. customdried
  10. distillationdistilled

Quellen und Nachweise

ORD-Eintrag
ord-b1fd55473c5449a3ab3e758cd1fe68cf
Quelldatensatz
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05633099

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