Lawesson's reagent → HCID 178481742, Verbindung

HRID 1598511Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1598511
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[C:13]1[CH:17]=[C:16](O)[N:15]([CH3:19])[N:14]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:29])=CC=1>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[C:13]1[CH:17]=[C:16]([SH:29])[N:15]([CH3:19])[N:14]=1

Komponenten

4

Edukt 2

HCID 87949Lawesson's reagentHCID 178481741HCID 178481741, Verbindung

Produkt 1

HCID 178481742HCID 178481742, VerbindungAusbeute 53 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A suspension of 1.0 g of 3-(2,6-dichloro-4-trifluoromethylphenyl)-5-hydroxy-1-methylpyrazole (6) and 0.7 g of Lawesson's reagent in 10 ml of toluene were refluxed with stirring for 3 hours. The solvent was distilled off under reduced pressure, and the resulting residue was purified by column chromatography on silica gel (eluent: ethyl acetate/hexane=1/6), giving 0.3 g of the desired compound in the form of colorless crystals (yield 27.3%).

Aufarbeitung

  1. temperaturewere refluxed
  2. distillationThe solvent was distilled off under reduced pressure
  3. customthe resulting residue was purified by column chromatography on silica gel (eluent: ethyl acetate/hexane=1/6)

Quellen und Nachweise

ORD-Eintrag
ord-8011d6b6e2624ecaa55b011a4993a01e
Quelldatensatz
uspto-grants-1998_04
Patentnummer
US05739083

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