Reaktion #61777

ord-070e2e793b2d4a3cb7bf238ab7b933c5

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, n-heptane, and ether
  7. 7
    SonstigeThe residue was dried at 40° C. in vacuum

Vorschrift

30 mg (0.74 mmol) of 60% sodium hydride were added to at 0° C. to a solution of 162 mg (0.70 mmol) 3-methyl-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 (0.70 mmol) 3-chloromethyl-2-methyl-6-(3-trifluoromethyl-phenyl)-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, n-heptane, and ether. The residue was dried at 40° C. in vacuum to give 255 mg (76%) of the title compound as slightly pink powder.

Quelle

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