Triphenylphosphine → HCID 90410612, compound

Participants

Reaction Steps

In a nitrogen atmosphere, 10.00 g of 2,6-difluoro-4-(4-propylphenyl)benzyl alcohol, 5.65 g of 3,4,5-trifluorophenol, and 13.01 g of triphenylphosphine were dissolved in 30 mL of THF, the resultant solution was cooled to −20° C., and 8.48 g of DIAD was added dropwise at such a rate that the inside temperature did not exceed −10° C. After stirring at room temperature for 1 hour, the solvent was distilled off under reduced pressure. Then, the residue was suspended by adding hexane, and precipitated triphenylphosphine was filtered off. An organic layer was washed with saturated brine and dried by adding sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography and then recrystallized from ethanol to yield 11.32 g of (3,4,5-trifluorophenyloxy)-[2,6-difluoro-4-(4-propylphenyl)phenyl]methane.

Provenance & Evidence