Reaktion #61759

ord-7b87ca582b674beab5ef911014819cc5

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    workup.STIRRINGstirring
  2. 2
    Sonstigecontinued at r.t overnight
  3. 3
    workup.STIRRINGwas stirred for 1 h
  4. 4
    Sonstigethe formed precipitate isolated by filtration
  5. 5
    Waschenwashed with water, methanol/water 1:1
  6. 6
    SonstigeThe residue was purified by chromatography on silica (eluent: ethyl acetate)

Vorschrift

8.0 mg (0.31 mmol) of 95% sodium hydride were added at 0° C. to a solution of 65 mg (0.28 mmol) 3-methyl-4-(4-[1,2,3]triazol-1-yl-butyl)-phenol in 3.0 ml N,N-dimethylformamide and stirred for 30 min. at 0° C. 76 mg (0.28 mmol) 2-chloromethyl-5-(4-trifluoromethyl-phenyl)-pyridine were given to the reaction mixture and stirring continued at r.t overnight. After addition of 6 ml water the mixture was stirred for 1 h, the formed precipitate isolated by filtration, washed with water, methanol/water 1:1. The residue was purified by chromatography on silica (eluent: ethyl acetate) to give 91 mg (70%) of the title compound as white powder.

Quelle

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