Lawesson's reagent → HCID 86649596, Verbindung

HRID 1530054Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1530054
[CH2:1]([N:3]1[CH:7]=[C:6]([C:8]([NH2:10])=O)[C:5]([CH3:11])=[N:4]1)[CH3:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:21])=CC=1>C1(C)C=CC=CC=1>[CH2:1]([N:3]1[CH:7]=[C:6]([C:8](=[S:21])[NH2:10])[C:5]([CH3:11])=[N:4]1)[CH3:2]

Komponenten

4

Edukt 2

HCID 87949Lawesson's reagentHCID 49949164HCID 49949164, Verbindung

Produkt 1

HCID 86649596HCID 86649596, VerbindungAusbeute 24 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a suspension of 1-ethyl-3-methyl-1H-pyrazole-4-carboxamide (1.7 g, 11 mmol) produced in the above in toluene (80 mL) was added Lawesson's reagent (7.0 g, 17 mmol), and the mixture was heated under reflux for 1.5 hr. The reaction solution was cooled to room temperature and purified by basic silica gel column chromatography (ethyl acetate/hexane=0/100→20/80) to give the title compound (445 mg, 24%) as a yellow oil.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1.5 hr
  3. custompurified by basic silica gel column chromatography (ethyl acetate/hexane=0/100→20/80)

Quellen und Nachweise

ORD-Eintrag
ord-c015e4199df84b3fa1780e2e724f026b
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09090601B2

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