反应详情

温度

30 °C

4-Butoxy-2,3-difluorophenol (24) (4.6 g) and tripotassium phosphate (K3PO4) (14.0 g) were added to DMF (100 ml) under a nitrogen atmosphere, and the stirring was continued at 70° C. The compound (20) (3.0 g) was added thereto, and the stirring was continued at 70° C. for 7 hours. After the reaction mixture obtained had been cooled to 30° C. and separated from solid materials by filtration, toluene (100 ml) and water (100 ml) were added thereto, and mixed. The mixture was then allowed to separate into organic and aqueous phases, and the extraction into an organic phase was carried out. The organic phase obtained was washed with brine and dried over anhydrous magnesium sulfate. Then, the solvent was distilled off, and the residue obtained was purified by means of column chromatography (silica gel; heptane/toluene=1/2 by volume). The product was further purified by means of recrystallization (Solmix A-11: heptane=1:2 by volume), giving 4.02 g of 2,3-difluoro-4-ethoxy-[trans-4-(2,3-difluoro-4-butoxyphenoxymethyl)cyclohexyl]benzene (No. 831). The yield based on the compound (20) was 85.1%.

1. customwas continued at 70° C
2. customAfter the reaction mixture obtained
3. customseparated from solid materials by filtration, toluene (100 ml) and water (100 ml)
4. additionwere added
5. additionmixed
6. customto separate into organic and aqueous phases
7. extractionthe extraction into an organic phase
8. customThe organic phase obtained
9. washwas washed with brine
10. dry with materialdried over anhydrous magnesium sulfate
11. distillationThen, the solvent was distilled off
12. customthe residue obtained
13. customwas purified by means of column chromatography (silica gel; heptane/toluene=1/2 by volume)
14. customThe product was further purified by means of recrystallization (Solmix A-11: heptane=1:2 by volume)