Dimethylformamide → HCID 54576351, Verbindung

HRID 1096946Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1096946
[C:1](=O)([O-])[O-].[K+].[K+].IC.CN(C=O)C.[OH:14][C:15]1[CH:16]=[C:17]([CH:22]=[C:23]([O:25][S:26]([C:29]([F:32])([F:31])[F:30])(=[O:28])=[O:27])[CH:24]=1)[C:18]([O:20][CH3:21])=[O:19]>C(OCC)C>[CH3:1][O:14][C:15]1[CH:16]=[C:17]([CH:22]=[C:23]([O:25][S:26]([C:29]([F:32])([F:30])[F:31])(=[O:28])=[O:27])[CH:24]=1)[C:18]([O:20][CH3:21])=[O:19]

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 86635508HCID 86635508, Verbindung

Produkt 1

HCID 54576351HCID 54576351, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

With cooling with ice, potassium carbonate (152 mg, 1.10 mmol) and iodomethane (0.137 mL, 2.20 mmol) were added to a DMF solution (3.0 mL) of methyl 3-hydroxy-5-trifluoromethane-sulfonyloxybenzoate (300 mg, 1.00 mmol), and stirred at room temperature for 17 hours. The reaction mixture was diluted with diethyl ether (30 mL), washed with water and aqueous saturated sodium chloride solution, dried with sodium sulfate, and concentrated under reduced pressure. The residue was purified through silica gel column chromatography to obtain the title compound as a colorless oil.

Aufarbeitung

  1. washwashed with water and aqueous saturated sodium chloride solution
  2. dry with materialdried with sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified through silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-49b0f8a3149c4f5b803e9a2a5fb9294a
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08138197B2

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