تفاعل #61773

ord-b86da0c3c75f4c76982d4cdbd522a431

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGstirring
  2. 2
    workup.WAITcontinued over night
  3. 3
    أخرىthe precipitate was isolated
  4. 4
    غسيلwashed thoroughly with water, methanol/water 1:1
  5. 5
    أخرىThe residue was purified by chromatography on silica (eluent: ethyl acetate/methanol 9:1)

الإجراء التجريبي

A solution of 126 mg (mmol) 4-(2-[1,2,3]triazol-1-yl-ethanesulfinylmethyl)-phenol in 4.0 ml N,N-dimethylformamide was treated at 0° C. with 14 mg (0.55 mmol) of 95% sodium hydride and stirred at 0° C. for 30 min., then 143 mg (0.50 mmol) 3-chloromethyl-2-methyl-6-(4-trifluoromethyl-phenyl)-pyridine were added and stirring continued over night. After addition of 8 ml water, the precipitate was isolated, washed thoroughly with water, methanol/water 1:1, and a small amount of ether. The residue was purified by chromatography on silica (eluent: ethyl acetate/methanol 9:1) to give 130 mg (52%) of the title compound as white powder.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07429605B2uspto-grants-2008_09