反応 #53294

反応方程式

1H-1,2,4-Triazole-3-thiol

triethylamine

2-Bromo-1-(4-(2,6-difluorobenzyloxy)phenyl)-1-Ethanone

→

title compound

3-(2-(4-(2,6-Difluorobenzyloxy)phenyl)-2-oxoethyl)thio-1H-1,2,4-triazole

溶媒

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   濃縮concentrated in vacuo
2. 2
   洗浄washed with 0.1M HCl, and brine
3. 3
   乾燥The organic layer was dried over Na2SO4
4. 4
   ろ過filtered
5. 5
   濃縮concentrated
6. 6
   その他purified by flash chromatography on silica gel column (chloroform:methanol, 9:1)

実験手順

To a solution of 1H-1,2,4-Triazole-3-thiol (0.250 g, 2.4 mmol) and triethylamine (2.50 g, 2.4 mmol) in dry dichloromethane (20 ml) was added 2-Bromo-1-(4-(2,6-difluorobenzyloxy)phenyl)-1-Ethanone (Step B, 0.851 g, 2.4 mmol) in dry dichloromethane (5 ml) at room temperature. The reaction mixture was stirred for 50 minutes and then concentrated in vacuo. The crude residue was taken in EtOAc and washed with 0.1M HCl, and brine. The organic layer was dried over Na2SO4, filtered, concentrated and purified by flash chromatography on silica gel column (chloroform:methanol, 9:1) to provide the title compound.

出典