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温度

0 °C

To a solution of triphenylphosphine (419 mg, 1.6 mmol) in anhydrous 20 mL DCM was added imidazole (224 mg, 3.3 mmol) and iodine (406 mg, 1.6 mmol) at 0° C. The reaction mixture was stirred for 30 min at 0° C. and then methyl 4-(4-fluorophenyl)-4-hydroxybutanoate (212 mg, 1 mmol) in 10 mL DCM was added to the mixture. The resulting mixture was stirred at 0° C. for 2 h and the temperature was slowly raised to room temp over a period of 3 h. Evaporation of solvent left the crude product as an oil from which the product was isolated by Flash column chromatography eluting with 0% to 10% ethyl acetate/hexane to give the title compound, 161 mg, as a light yellow oil.

1. stirringThe resulting mixture was stirred at 0° C. for 2 h
2. temperaturethe temperature was slowly raised to room temp over a period of 3 h
3. customEvaporation of solvent
4. waitleft the crude product as an oil from which the product
5. customwas isolated by Flash column chromatography
6. washeluting with 0% to 10% ethyl acetate/hexane