反应 #90322

ord-a1c8ac62b26b460c9c80443c7658ff7d

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The mixture was quenched with aqueous ammonium chloride
  2. 2
    萃取extracted with ethyl acetate
  3. 3
    干燥The organic layer was dried over magnesium sulfate
  4. 4
    过滤filtered
  5. 5
    浓缩concentrated
  6. 6
    其他The residue was purified via radial chromatography

实验过程

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%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09445594B2uspto-grants-2016_09