反应详情

3.5 g of 2-hydroxy-4-(5-fluoro-2-methoxyphenyl)-4-methyl-2-trifluoromethyl-pentanol and 3.45 g of triphenylphosphine are dissolved in 50 ml of tetrahydrofuran and mixed in 3 portions at 0° C. with 2.5 ml of azodicarboxylic acid-diethyl ester. After one hour at 0° C., it is stirred for 16 more hours at room temperature, then refluxed for 7 hours and again stirred for 48 hours at room temperature. After concentration by evaporation, a hexane-isopropylether mixture is added, filtered, and the filtrate is chromatographed on silica gel. The product that is eluted with hexane/ethyl acetate is distilled on a bulb tube, boiling point 100° C./0.5 mbar.

1. temperaturerefluxed for 7 hours
2. stirringagain stirred for 48 hours at room temperature
3. concentrationAfter concentration
4. customby evaporation
5. additiona hexane-isopropylether mixture is added
6. filtrationfiltered
7. customthe filtrate is chromatographed on silica gel
8. washThe product that is eluted with hexane/ethyl acetate
9. distillationis distilled on a bulb tube