반응 #48701

반응 방정식

trifluoromethanesulphonic anhydride

2-fluoro-2-methylpropan-1-ol

2,6-lutidine

→

desired compound

수율 70.0%

Trifluoromethanesulfonic acid 2-fluoro-2-methylpropyl ester

수율 70.0%

용매

dichloromethane

반응 조건

후처리

1. 1
   기타Add water to quench
2. 2
   기타the reaction
3. 3
   기타separate the organic layer
4. 4
   추출extract the aqueous layer with dichloromethane
5. 5
   건조dry (magnesium sulfate)
6. 6
   여과filter
7. 7
   농축concentrate
8. 8
   기타purify
9. 9
   세척(silica gel chromatography, eluting with dichloromethane)

실험 절차

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).

출처