2,4'-Dichloroacetophenone → 2-(4-Chlorophenyl)-2-oxoethyl thiocyanate

HRID 604874

Reaktionsgleichung

Reaktionsgleichung von HRID 604874
Cl[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][CH:6]=1)=[O:4].[C:12]([S-:14])#[N:13].[K+]>>[Cl:11][C:8]1[CH:9]=[CH:10][C:5]([C:3](=[O:4])[CH2:2][S:14][C:12]#[N:13])=[CH:6][CH:7]=1

Komponenten

3

Edukt 2

HCID 702982,4'-DichloroacetophenoneHCID 516872Potassium thiocyanate

Produkt 1

HCID 880132-(4-Chlorophenyl)-2-oxoethyl thiocyanateAusbeute 90 %

Versuchsvorschrift

A solution of 945 mg (5 mmol) 2,4′-dichloroacetophenone and 583 mg (6 mmol) potassium rhodanide was heated to reflux for 30 minutes. After a few minutes a precipitation was formed. The solvent was evaporated under reduced pressure and the residue was suspended in tetrahydrofurane, stirred for 1 hour at room temperature, filtered and the filtrate was concentrated in vacuo. The residue was stirred with heptane and little ethanol for 15 minutes. The product was filtered off and dried to yield 953 mg (90%) 1-(4-chloro-phenyl)-2-thiocyanato-ethanone as a light yellow solid. 1H NMR (CDCl3, 250 MHz): δ (ppm)=7.89 (d, 2H), 7.51 (d, 2H), 4.692 (s, 2H).

Aufarbeitung

  1. temperatureto reflux for 30 minutes
  2. customAfter a few minutes a precipitation
  3. customwas formed
  4. customThe solvent was evaporated under reduced pressure
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated in vacuo
  7. stirringThe residue was stirred with heptane and little ethanol for 15 minutes
  8. filtrationThe product was filtered off
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-f236601bf5e449eeadf020241375a1af
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07910740B2

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