Reaktion #61761

ord-897976c5894045cf8f739b6b2729e2d4

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, methanol/water 1:1
  7. 7
    SonstigeThe residue was purified by chromatography on silica (eluent: ethyl acetate/n-heptane 4:1)

Vorschrift

15 mg (0.60 mmol) of 95% sodium hydride were added at 0° C. to a solution of 116 mg (0.50 mmol) 3-methyl-4-(4-[1,2,3]triazol-1-yl-butyl)-phenol in 4.0 ml N,N-dimethylformamide and stirred for 30 min. at 0° C. 144 mg (0.50 mmol) 5-chloromethyl-2-(4-trifluoromethoxy-phenyl)-pyridine were given to the reaction mixture and stirring continued at room temperature (r.t.) overnight. After addition of 8 ml water the mixture was stirred for 1 h, the formed precipitate isolated by filtration, washed with water, methanol/water 1:1, and a small amount of ether. The residue was purified by chromatography on silica (eluent: ethyl acetate/n-heptane 4:1) to give 136 mg (56%) of the title compound as white powder.

Quelle

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