反应详情

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).

1. customAdd water to quench
2. customthe reaction
3. customseparate the organic layer
4. extractionextract the aqueous layer with dichloromethane
5. dry with materialdry (magnesium sulfate)
6. filtrationfilter
7. concentrationconcentrate
8. custompurify
9. wash(silica gel chromatography, eluting with dichloromethane)