反应详情

To a solution of triphenylphosphine(2 eq) in dichloromethane at 0° C. under nitrogen was added dropwise triflic anhydride(1 eq). After 15 minutes 2-(2-fluoro-5-nitrophenyl)-2-methylbutane-1,4-diol(1 eq)was added in dichloromethane followed by potassium carbonate(1 eq). The resulting mixture was allowed to warm to room temperature for 5 h. To the mixture was added water and extracted with dichloromethane. The organic layer was washed with brine and dried with sodium sulfate and concentrated. Crude product was purified using flash chromatography (85% Hex:15% EtoAc) on silica to afford 3-(2-fluoro-5-nitrophenyl)-tetrahydro-3-methylfuran.

1. extractionextracted with dichloromethane
2. washThe organic layer was washed with brine
3. dry with materialdried with sodium sulfate
4. concentrationconcentrated
5. customCrude product was purified