反応 #501282

反応方程式

2-(2,6-difluorophenyl)propan-2-ol

hydrazoic acid

trifluoroacetic acid

→

2-(2,6-difluorophenyl)-2-azidopropane

溶媒

hexane

反応条件

後処理

1. 1
   洗浄washed with water
2. 2
   乾燥with sodium bicarbonate until free of acid and dried over sodium sulfate
3. 3
   その他The solvent is removed by evaporation
4. 4
   workup.DISTILLATIONthe residue is distilled

実験手順

20.6 g (120 millimoles) of 2-(2,6-difluorophenyl)propan-2-ol are dissolved in 300 ml of hydrazoic acid solution (1N, in benzene) and 22.8 g (200 millimoles) of trifluoroacetic acid are added to this solution. After 24 hours at room temperature, the reaction solution is diluted with 500 ml of hexane, washed with water and then with sodium bicarbonate until free of acid and dried over sodium sulfate. The solvent is removed by evaporation and the residue is distilled, affording 2-(2,6-difluorophenyl)-2-azidopropane of bp15 =85°-87° C.

出典