Реакция #61763

ord-c2ef141466b346a2b2f6a9fee83c5f5d

Растворители

Условия реакции

Температура
0°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.STIRRINGstirring
  2. 2
    Другоеcontinued at room temperature
  3. 3
    Другое(r.t.) overnight
  4. 4
    workup.STIRRINGwas stirred for 1 h
  5. 5
    Другоеthe formed precipitate isolated by filtration
  6. 6
    Промывкаwashed with water, water/methanol 1:1, and ether
  7. 7
    ДругоеThe residue was purified by chromatography on silica (eluent: ethyl acetate)

Методика

36 mg (0.90 mmol) of 95% sodium hydride were added to at 0° C. to a solution of 173 mg (0.75 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. 214 mg (0.75 mmol) 3-chloromethyl-2-methyl-6-(4-trifluoromethyl-phenyl)-pyridine (WO 2005/049573) 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, water/methanol 1:1, and ether. The residue was purified by chromatography on silica (eluent: ethyl acetate) to yield 227 mg (63%) of the title compound as white crystals.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07429605B2uspto-grants-2008_09