反応 #48701

反応方程式

trifluoromethanesulphonic anhydride

2-fluoro-2-methylpropan-1-ol

2,6-lutidine

→

desired compound

収率 70.0%

Trifluoromethanesulfonic acid 2-fluoro-2-methylpropyl ester

収率 70.0%

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他Add water to quench
2. 2
   その他the reaction
3. 3
   その他separate the organic layer
4. 4
   抽出extract the aqueous layer with dichloromethane
5. 5
   乾燥dry (magnesium sulfate)
6. 6
   ろ過filter
7. 7
   濃縮concentrate
8. 8
   その他purify
9. 9
   洗浄(silica gel chromatography, eluting with dichloromethane)

実験手順

Add trifluoromethanesulphonic anhydride (4.3 mL, 26.0 mmol) to a solution of 2-fluoro-2-methylpropan-1-ol (2.0 g, 21.7 mmol) and 2,6-lutidine (3.0 mL, 26.0 mmol) in dichloromethane (25 mL) at −78° C. Warm slowly to room temperature and stir at room temperature for 1 hour. Add water to quench the reaction, separate the organic layer and extract the aqueous layer with dichloromethane. Combine the organic layers, dry (magnesium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with dichloromethane), to give the desired compound as an oil (3.4 g, 70% yield).

出典