反应详情

To a solution of n-decanol (1.6 g) and 4-methylcarbonyloxy-4'-carboxybiphenyl (2.6 g) in tetrahydrofuran (50 ml) were added dicyclohexylcarbodiimide (1.4 g) and dimethylaminopyridine (0.5 g), followed by stirring at room temperature for 24 hours. Thereto was added tert-butylamine and the mixture was refluxed at 70° C. for 2 hours and hydrolyzed. After the solvent was distilled off, dilute hydrochloric acid was added to make the solution neutral and the solution was extracted with diethyl ether. After the solvent was distilled off, the residue was washed with hexane and recrystallized from water/ethanol (1/9) solution to obtain the titled compound (about 2.3 g).

1. temperaturethe mixture was refluxed at 70° C. for 2 hours
2. distillationAfter the solvent was distilled off
3. additiondilute hydrochloric acid was added
4. extractionthe solution was extracted with diethyl ether
5. distillationAfter the solvent was distilled off
6. washthe residue was washed with hexane
7. customrecrystallized from water/ethanol (1/9) solution