1-(3-Chloro-4-nitrophenyl)ethanone → 3'-(2,4-Difluorophenylthio)-4'-nitroacetophenone

HRID 1087192Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1087192
Cl[C:2]1[CH:3]=[C:4]([C:11](=[O:13])[CH3:12])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].[F:14][C:15]1[CH:21]=[C:20]([F:22])[CH:19]=[CH:18][C:16]=1[S-:17].[K+]>C1(C)C(C)=CC=CC=1>[F:14][C:15]1[CH:21]=[C:20]([F:22])[CH:19]=[CH:18][C:16]=1[S:17][C:2]1[CH:3]=[C:4]([C:11](=[O:13])[CH3:12])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9]

Komponenten

4

Edukt 2

HCID 104427551-(3-Chloro-4-nitrophenyl)ethanoneHCID 23700122Potassium 2,4-difluorothiophenoxide

Produkt 1

HCID 102448083'-(2,4-Difluorophenylthio)-4'-nitroacetophenoneAusbeute 61,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

A mixture of 3'-chloro-4'-nitroacetophenone (2.4 g), potassium 2,4-difluorothiophenoxide (2.7 g), and N,Ndimethylformamide (5 ml) in xylene (50 ml) was stirred for 8 hours at room temperature. The mixture was poured into ice-water and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The residual solid was recrystallized from ethanol to give prisms of 3'-(2,4-difluorophenylthio)-4'-nitroacetophenone (2.3 g).

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residual solid was recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-32a801e5fbff4ed1a50c02c93b95d056
Quelldatensatz
uspto-grants-1991_07
Patentnummer
US05034417

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