反应详情

温度

70 °C

(4-(6-Propyldecahydronaphthalene-2-yl)cyclohexyl)methyl p-toluenesulfonate (3.5 g) prepared in the tenth step was dissolved in DMF (50 ml). 4-Ethoxy-2,3-difluorophenol (1.6 g) and potassium carbonate (2.2 g) were added, and the mixture was stirred at 70° C. for 5 hours. The reaction mixture was washed with water, and dried over anhydrous magnesium sulfate. The DMF was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: ethyl acetate/n-heptane=1/20 by volume) and then by recrystallization (solvent: Solmix/n-heptane=1/4 by volume) to give 2-(4-((4-ethoxy-2,3-difluorophenoxy)methyl)cyclohexyl)-6-propyldecahydronaphthalene (2.1 g).

1. washThe reaction mixture was washed with water
2. dry with materialdried over anhydrous magnesium sulfate
3. distillationThe DMF was distilled off under reduced pressure
4. customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate/n-heptane=1/20 by volume)
5. customby recrystallization (solvent: Solmix/n-heptane=1/4 by volume)