1-Bromo-2-Chloroethane → (2-Chloroethyl)-(3,4-difluorophenyl)sulfane

HRID 660048Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 660048
Br[CH2:2][CH2:3][Cl:4].C([O-])([O-])=O.[K+].[K+].[F:11][C:12]1[CH:13]=[C:14]([SH:19])[CH:15]=[CH:16][C:17]=1[F:18]>CN(C=O)C.CC(=O)OCC>[Cl:4][CH2:3][CH2:2][S:19][C:14]1[CH:15]=[CH:16][C:17]([F:18])=[C:12]([F:11])[CH:13]=1

Komponenten

6

Edukt 3

HCID 78491-Bromo-2-ChloroethaneHCID 11430Potassium CarbonateHCID 27783783,4-Difluorobenzenethiol

Produkt 1

HCID 43236186(2-Chloroethyl)-(3,4-difluorophenyl)sulfaneAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

5.7 ml (68.4 mmol) of 1-bromo-2-chloroethane and 1.9 g (13.7 mmol) of K2CO3 were added to a solution of 2.0 g (13.7 mmol) of 3,4-difluorothiophenol in DMF (20 ml). Stirring was then carried out for 5 h at 60° C. and for 16 h at RT. The mixture was then diluted with EA (50 ml) and washed in succession with 1 M aq. Na2CO3 solution and brine. The organic phase was dried over MgSO4, filtered and concentrated in vacuo. There were obtained as residue 2.7 g (12.9 mmol, 95%) of (2-chloroethyl)-(3,4-difluorophenyl)sulfane, which was reacted further without additional purification.

Aufarbeitung

  1. washwashed in succession with 1 M aq. Na2CO3 solution and brine
  2. dry with materialThe organic phase was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-bb0d275f173041d1a63f9b9e7d608c88
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08084470B2

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