Water → 1-(Methylthio)-2-(trifluoromethoxy)benzene

HRID 412447Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 412447
CI.[C:3](=O)([O-])[O-].[K+].[K+].[F:9][C:10]([F:20])([F:19])[O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[SH:18].O>CN(C=O)C>[CH3:3][S:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[O:11][C:10]([F:9])([F:19])[F:20]

Komponenten

6

Edukt 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 27607322-(Trifluoromethoxy)thiophenol

Produkt 1

HCID 27815671-(Methylthio)-2-(trifluoromethoxy)benzeneAusbeute 90,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of methyl iodide (59.0 g, 0.41 mol) in DMF (150 mL) was added potassium carbonate (23.0 g, 0.16 mol). 2-(Trifluoromethoxy)thiophenol (16.0 g, 0.08 mol) was added in portions during 30 min. The reaction mixture was then stirred vigorously overnight. Water (250 mL) was added. The reaction mixture was extracted with ethyl acetate (2×150 mL). The combined organic phases were washed with a 50% saturated aqueous solution of sodium chloride (4×100 mL), dried (magnesium sulphate), and concentrated in vacuo to give 15.0 g of 1-methylsulfanyl-2-trifluoromethoxybenzene.

Aufarbeitung

  1. extractionThe reaction mixture was extracted with ethyl acetate (2×150 mL)
  2. washThe combined organic phases were washed with a 50% saturated aqueous solution of sodium chloride (4×100 mL)
  3. dry with materialdried (magnesium sulphate)
  4. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-7c2d53f115284b089a8846ed368d83cd
Quelldatensatz
uspto-grants-2003_05
Patentnummer
US06562807B2

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