反应详情

To a solution of 4'-(1,1,1-trifluoro-2-octyloxycarbonyl)biphenyl-4-carbonylchloride (1.3 g) and 4-n-octyloxyphenol (1.0 g) in methylene chloride (40 ml) were added triethylamine (0.5 g) and dimethylaminopyridine (0.032 g). The mixture was stirred for 24 hours at room temperature before it was poured in water. Extraction was made with methylene chloride and the extract was washed with dilute aqueous sodium carbonate solution and water, in this order and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by silica gel column chromatography (developer hexane ethyl acetate 10 0.5) and recrystallized from ethanol to obtain the titled compound (0.8 g).

1. extractionExtraction
2. washthe extract was washed with dilute aqueous sodium carbonate solution and water, in this order
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationAfter the solvent was distilled off
5. customthe residue was purified by silica gel column chromatography (developer hexane ethyl acetate 10 0.5)
6. customrecrystallized from ethanol