Реакция #61779

ord-78f0c2c4f1d44a5e887443c0e9085bfc

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

Методика

28 mg (0.69 mmol) of 60% sodium hydride were added to at 0° C. to a solution of 153 mg (0.66 mmol) 3-methyl-4-(4-[1,2,3]triazol-1-yl-butyl)-phenol in 6.0 ml N,N-dimethylformamide and stirred for 30 min. at 0° C. 200 mg (0.66 mmol) 3-chloromethyl-2-methyl-6-(3-trifluoromethoxy-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 234 mg (72%) of the title compound as slightly yellow powder.

Источник

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