Reaktion #420253

ord-e156cebccf7442b09023dbb494268048

Lösungsmittel

Reaktionsbedingungen

Temperatur
160°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigepurified by column chromatography (silica, ethyl acetate/methanol, 1% concentrated NH3)

Vorschrift

N-(2-Chloro-6-methyl-4-pyridyl)ethane-1,2-diamine (0.205 g, 1.2 mmol) was combined with the sodium salt of 2-methylbutan-1-ol (0.66 g, 6 mmol, that had been obtained by treating 2-methylbutan-1-ol with sodium hydride dispersion in THF), diphenylether (2.2 g) and DMSO (0.75 ml). The mixture was heated at 160° C. for 16 hours and purified by column chromatography (silica, ethyl acetate/methanol, 1% concentrated NH3) to yield 200 mg of a brown oil (0.84 mmol, 70%). MS (APCI) m/z=237.9 [M+1]+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08877934B2uspto-grants-2014_11