Lawesson's reagent → 1-(Pyridazin-3-yl)ethan-1-ol

HRID 1503427Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1503427
CON(C)[C:4]([C:6]1[N:7]=[N:8][CH:9]=[CH:10][CH:11]=1)=[O:5].[CH3:13]OC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=S)=CC=1>C1(C)C=CC=CC=1>[N:8]1[CH:9]=[CH:10][CH:11]=[C:6]([CH:4]([OH:5])[CH3:13])[N:7]=1

Komponenten

4

Edukt 2

HCID 87949Lawesson's reagentHCID 58197546N-methoxy-N-methylpyridazine-3-carboxamide

Produkt 1

HCID 151975111-(Pyridazin-3-yl)ethan-1-olAusbeute 193,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

A suspension of compound 2 (180 mg, 0.4 mmol) and Lawesson's Reagent (180 mg, 0.44 mmol) in dry toluene (4 mL) was heated under 130° C. for 35 min in a CEM microwave reactor. The mixture was concentrated in vacuo and the residue was purified by column (eluent:petroleum ether:ethyl acetate=5:1) to give compound 3 as a white solid (96 mg, 50%) as a white solid.

Aufarbeitung

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue was purified by column (eluent:petroleum ether:ethyl acetate=5:1)

Quellen und Nachweise

ORD-Eintrag
ord-57c78b1a087642259a82a263dd17cf47
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09212153B2

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