反応 #61785

ord-0a1503599fa9477d8024684024b47c92

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGstirring
  2. 2
    その他continued at r.t overnight
  3. 3
    workup.STIRRINGwas stirred for 1 h
  4. 4
    その他the formed precipitate isolated by filtration
  5. 5
    洗浄washed with water, methanol/water 1:1
  6. 6
    その他The residue was dried at 40° C.

実験手順

16 mg (0.39 mmol) of 95% sodium hydride were added at 0° C. to a solution of 86 mg (0.37 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. 100 mg (0.37 mmol) 2-chloromethyl-6-(4-trifluoromethyl-phenyl)-pyridine were given to the reaction mixture and stirring continued at 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 dried at 40° C. to give 145 mg (84%) of the title compound as white powder.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07429605B2uspto-grants-2008_09