Reaktion #61782

ord-b9ad8d85400949f199a488ba0a5883d2

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGstirring
  2. 2
    Sonstigecontinued at room temperature
  3. 3
    Sonstige(r.t.) overnight
  4. 4
    workup.STIRRINGwas stirred for 1 h
  5. 5
    Sonstigethe formed precipitate isolated by filtration
  6. 6
    Waschenwashed with water, water/methanol 1:1, and ether
  7. 7
    SonstigeThe residue was dried at 40° C. in vacuum

Vorschrift

36 mg (0.89 mmol) of 60% sodium hydride were added to at 0° C. to a solution of 185 mg (0.85 mmol) 4-(4-[1,2,3]triazol-1-yl-butyl)-phenol in 8.0 ml N,N-dimethylformamide and stirred for 30 min. at 0° C. 200 mg (0.85 mmol) 3-chloromethyl-6-(4-fluoro-phenyl)-2-methyl-pyridine were given to the reaction mixture and stirring continued at room temperature (r.t.) overnight. After addition of 16 ml water the mixture was stirred for 1 h, the formed precipitate isolated by filtration, washed with water, water/methanol 1:1, and ether. The residue was dried at 40° C. in vacuum to give 295 mg (83%) of the title compound as white powder.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07429605B2uspto-grants-2008_09