Реакция #61784

ord-cbad8edbeb3c4836b5af369697c463a0

Растворители

Условия реакции

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

Обработка

  1. 1
    workup.STIRRINGstirring
  2. 2
    workup.WAITcontinued at r.t for 2 days
  3. 3
    workup.STIRRINGwas stirred for 1 h
  4. 4
    Другоеthe formed precipitate isolated by filtration
  5. 5
    Промывкаwashed with water, methanol/water 1:1
  6. 6
    ДругоеThe residue was dried at 40° C.

Методика

16 mg (0.39 mmol) of 60% sodium hydride were added at 0° C. to a solution of 80 mg (0.37 mmol) 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. 100 mg (0.37 mmol) 2-chloromethyl-6-(4-trifluoromethyl-phenyl)-pyridine (WO 2004/007439) were given to the reaction mixture and stirring continued at r.t for 2 days. 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 dried at 40° C. to give 101 mg (60%) of the title compound as white powder.

Источник

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