Ethanethiol → HCID 91876372, Verbindung

HRID 1052926Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1052926
[CH2:1]([SH:3])[CH3:2].F[C:5]1[CH:13]=[C:12]([C:14]([F:17])([F:16])[F:15])[CH:11]=[CH:10][C:6]=1[C:7]([OH:9])=[O:8].C(=O)([O-])[O-].[Cs+].[Cs+].C(=O)(O)[O-].[Na+]>CN1C(=O)CCC1>[CH2:1]([S:3][C:5]1[CH:13]=[C:12]([C:14]([F:15])([F:17])[F:16])[CH:11]=[CH:10][C:6]=1[C:7]([OH:9])=[O:8])[CH3:2]

Komponenten

6

Edukt 4

HCID 6343EthanethiolHCID 10796Cesium carbonateHCID 516892Sodium BicarbonateHCID 5180032-Fluoro-4-(trifluoromethyl)benzoic acid

Produkt 1

HCID 91876372HCID 91876372, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

1.5 mL of ethyl mercaptan was added to a mixture of 3.83 g of 2-fluoro-4-trifluoromethylbenzoic acid, 10 mL of NMP and 15 g of cesium carbonate, and the mixture was stirred at 60° C. for 4 hours. A saturated aqueous sodium bicarbonate solution was added to the cooled reaction mixture, and the mixture was extracted with ethyl acetate. Hydrochloric acid was added to the aqueous layer, and the precipitated solid was taken by filtration and dried under reduced pressure to obtain 4.6 g of 2-ethylsulfanyl-4-trifluoromethylbenzoic acid.

Aufarbeitung

  1. extractionthe mixture was extracted with ethyl acetate
  2. additionHydrochloric acid was added to the aqueous layer
  3. filtrationthe precipitated solid was taken by filtration
  4. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-05a4ebb12e1748c8b60144b170c19cf8
Quelldatensatz
uspto-grants-2016_07
Patentnummer
US09392791B2

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