Cesium carbonate → HCID 57930950, Verbindung

HRID 1096982Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1096982
C(=O)([O-])[O-].[Cs+].[Cs+].[Br:7][C:8]1[C:17]([O:18][S:19]([C:22]([F:25])([F:24])[F:23])(=[O:21])=[O:20])=[CH:16][C:11]([C:12]([O:14][CH3:15])=[O:13])=[CH:10][C:9]=1[O:26]S(C(F)(F)F)(=O)=O>COCCOC>[Br:7][C:8]1[C:17]([O:18][S:19]([C:22]([F:23])([F:24])[F:25])(=[O:20])=[O:21])=[CH:16][C:11]([C:12]([O:14][CH3:15])=[O:13])=[CH:10][C:9]=1[OH:26]

Komponenten

4

Edukt 2

HCID 10796Cesium carbonateHCID 57930942HCID 57930942, Verbindung

Produkt 1

HCID 57930950HCID 57930950, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 80711,2-DimethoxyethaneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

In a 1-liter egg plant-type flask, cesium carbonate (24.8 g, 76.3 mmol) was added to a DME (200 mL) solution of methyl 4-bromo-3,5-bis{[(trifluoromethyl)sulfonyl]oxy}benzoate (26.0 g), and stirred at 60° C. for 3 hours. DME was removed under reduced pressure, the residue was diluted with ethyl acetate, washed with water and saturated saline water in that order, dried with sodium sulfate, filtered and concentrated to obtain a crude product as a brown solid. This was washed with a mixed solvent of toluene and hexane to obtain the title compound as a colorless solid.

Aufarbeitung

  1. customDME was removed under reduced pressure
  2. additionthe residue was diluted with ethyl acetate
  3. washwashed with water and saturated saline water in that order
  4. dry with materialdried with sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto obtain a crude product as a brown solid
  8. washThis was washed with a mixed solvent of toluene and hexane

Quellen und Nachweise

ORD-Eintrag
ord-74ac28e307c243658e3d40f7cb5af923
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08138197B2

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