반응 #90322

ord-a1c8ac62b26b460c9c80443c7658ff7d

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixture was quenched with aqueous ammonium chloride
  2. 2
    추출extracted with ethyl acetate
  3. 3
    건조The organic layer was dried over magnesium sulfate
  4. 4
    여과filtered
  5. 5
    농축concentrated
  6. 6
    기타The residue was purified via radial chromatography

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09445594B2uspto-grants-2016_09