تفاعل #90322

ord-a1c8ac62b26b460c9c80443c7658ff7d

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    أخرىThe mixture was quenched with aqueous ammonium chloride
  2. 2
    استخلاصextracted with ethyl acetate
  3. 3
    تجفيفThe organic layer was dried over magnesium sulfate
  4. 4
    ترشيحfiltered
  5. 5
    تركيزconcentrated
  6. 6
    أخرىThe residue was purified via radial chromatography

الإجراء التجريبي

To N-(4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)acetamide in tetrahydrofuran (1.1 mL) cooled to −78° C. was added n-butyllithium (2.5 M, 0.13 mL). The reaction was stirred for 1 hour. 1-Isothiocyanato-3-methylbenzene was added and the solution was slowly warmed to 0° C. over 1 hour. The mixture was quenched with aqueous ammonium chloride and extracted with ethyl acetate. The organic layer was dried over magnesium sulfate, filtered, and concentrated. The residue was purified via radial chromatography using a 97:3 chloroform/methanol mixture as eluent providing the title compound as a tan solid (0.062 g, 55%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09445594B2uspto-grants-2016_09