反応 #2155

反応方程式

1-Phenyl-2-propyn-1-ol

2,6-Lutidine

tert-butyldimethylsilyl trifluoromethane sulfonate

→

title compound

tert-Butyldimethylsilyloxy-1-phenyl-prop-1-yne

溶媒

dichloromethane

反応条件

後処理

1. 1
   洗浄The dichloromethane was washed with water (2×), brine
2. 2
   乾燥dried (MgSO4) and solvent
3. 3
   その他removed in vacuo
4. 4
   その他The residue was purified on flash silica using 100% petrol moving to 5% ethyl acetate/petrol

実験手順

1-Phenyl-2-propyn-1-ol (7 g) was dissolved in dichloromethane at 0° C. under nitrogen. 2,6-Lutidine (6.17 ml) was added to the solution followed by dropwise addition of tert-butyldimethylsilyl trifluoromethane sulfonate (12.16 ml); the resulting solution was stirred overnight at room temperature. The dichloromethane was washed with water (2×), brine and dried (MgSO4) and solvent removed in vacuo. The residue was purified on flash silica using 100% petrol moving to 5% ethyl acetate/petrol, to afford the title compound as a yellow oil (10.31 g).

出典