反応 #90322

反応方程式

N-(4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)acetamide

n-butyllithium

1-Isothiocyanato-3-methylbenzene

→

title compound

収率 55.0%

N-(m-tolylcarbamothioyl)-N-(4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)acetamide

収率 55.0%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   その他The mixture was quenched with aqueous ammonium chloride
2. 2
   抽出extracted with ethyl acetate
3. 3
   乾燥The organic layer was dried over magnesium sulfate
4. 4
   ろ過filtered
5. 5
   濃縮concentrated
6. 6
   その他The residue was purified via radial chromatography

実験手順

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%).

出典