反应详情

温度

80 °C

0.391 g of thionyl chloride and 0.104 g of pyridine were added to toluene (3 g) solution of 0.3 g of 1-(4-bromo-3-methylphenyl)-3-(3,5-dichlorophenyl)-3-hydroxy-4,4,4-trifluorobutan-1-one synthesized in Step 3 at room temperature and stirred for 1 hour at 80° C. After completion of the reaction, the reaction solution was cooled to room temperature, and separated by adding toluene and 2N hydrochloric acid. The organic phase was washed with water, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. Although the obtained residue includes a mixture of geometric isomers, this residue was purified by silica gel column chromatography which eluted the residue with ethyl acetate-hexane (1:10) to obtain 0.244 g of the target product as a yellow solid.

1. customAfter completion of the reaction
2. temperaturethe reaction solution was cooled to room temperature
3. customseparated
4. additionby adding toluene and 2N hydrochloric acid
5. washThe organic phase was washed with water
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationThe solvent was distilled off under reduced pressure
8. additiona mixture of geometric isomers
9. customthis residue was purified by silica gel column chromatography which
10. washeluted the residue with ethyl acetate-hexane (1:10)