Dimethylformamide → HCID 59593959, compound

Participants

Reaction Conditions

Reaction Steps

In a reactor 4.0 g of compound (a4), 5.3 g of compound (a6) and 1.2 g of potassium hydroxide (KOH) were added into 30 ml of N,N-dimethylformamide (DMF), and stirred at 60° C. for 14 hours. The reaction mixture was cooled to 30° C., to which 100 ml of water and 100 ml of toluene were added. The mixture was allowed to separate into organic layer and aqueous layer and the organic layer was extracted. The resulting organic layer was separated and washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to provide the residue. The resulting residue was purified by column chromatography (silica gel; toluene), further purified by re-crystallization from (volume ratio Solmix A-11: toluene=1:2), and dried to provide 2.5 g of 4′-ethoxy-2,3,2′,3′-tetrafluoro-4-(4′-vinylbicyclohexyl-4-ylmetoxy)-biphenyl (a7).

Provenance & Evidence