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2,4-Difluorobenzonitrile → 4-Fluoro-2-(methylsulfanyl)benzonitrile

HRID 897362
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 897362
F[C:2]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[CH3:11][S-:12]>C(Cl)Cl>[F:10][C:8]1[CH:7]=[CH:6][C:3]([C:4]#[N:5])=[C:2]([S:12][CH3:11])[CH:9]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 775452,4-DifluorobenzonitrileHCID 519392Mercaptomethanide

Produkt 1

HCID 167539444-Fluoro-2-(methylsulfanyl)benzonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

2,4-difluorobenzonitrile (2.0 g, 14.38 mmol) and thiomethoxide (1.02 g, 14.38 mmol) were placed in an oven dried 100 mL round bottom flask fitted with a reflux condenser. Toluene (40 mL) was added and the reaction solution was put under an atmosphere of Argon. The reaction was heated to 90 deg C. over 48 hours. The crude reaction was cooled and concentrated in vacuo. The residue was taken up in methylene chloride and extracted with water. The organic phase was dried (MgSO4), filtered and concentrated to afford a white solid. The solid was dissolved in a minimal amount of methylene chloride and purified on an ISCO column (110 g silica) with a gradient of 100% hexanes to 80% hexanes/20% ethylacetate over 15 min, then 20% EtOAc/80% Hexanes for 5 min. The collected fractions were evaporated in vacuo to afford the desired material in a 7.5:1 ratio 4-fluoro-2-(methylthio)benzonitrile: 2-fluoro-4-(methylthio)benzonitrile. The white solid was carried on to the next step without further purification.

Aufarbeitung

  1. customdried 100 mL round bottom flask
  2. customfitted with a reflux condenser
  3. additionToluene (40 mL) was added
  4. temperatureThe reaction was heated to 90 deg C
  5. customThe crude reaction
  6. temperaturewas cooled
  7. concentrationconcentrated in vacuo
  8. extractionextracted with water
  9. dry with materialThe organic phase was dried (MgSO4)
  10. filtrationfiltered
  11. concentrationconcentrated
  12. customto afford a white solid
  13. custompurified on an ISCO column (110 g silica) with a gradient of 100% hexanes to 80% hexanes/20% ethylacetate over 15 min
  14. wait20% EtOAc/80% Hexanes for 5 min
  15. customThe collected fractions were evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-1d95d791a3d74829ae7de0a0d9e9a11b
Quelldatensatz
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06921759B2

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