Reacción #48701

Ecuación de reacción

trifluoromethanesulphonic anhydride

2-fluoro-2-methylpropan-1-ol

2,6-lutidine

→

desired compound

Rendimiento 70.0%

Trifluoromethanesulfonic acid 2-fluoro-2-methylpropyl ester

Rendimiento 70.0%

Disolventes

dichloromethane

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroAdd water to quench
2. 2
   Otrothe reaction
3. 3
   Otroseparate the organic layer
4. 4
   Extracciónextract the aqueous layer with dichloromethane
5. 5
   Secadodry (magnesium sulfate)
6. 6
   Filtraciónfilter
7. 7
   Concentraciónconcentrate
8. 8
   Otropurify
9. 9
   Lavado(silica gel chromatography, eluting with dichloromethane)

Procedimiento

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).

Fuente