反应详情

0.55 g (2.01 mM of 2-octylindan-5-boronic acid, 0.80 g (1.81 mM) of 4-(4-decylphenyl)phenyl triflate, 1.5 ml of ethanol, 2.8 ml of toluene, 2.8 ml of 2M-sodium carbonate aqueous solution and 0.09 g of tetrakis(triphenylphosphine)palladium (O) were mixed and heat-refluxed for 4 hours under stirring. After the reaction, the reaction mixture, water and toluene were added to followed by filtration under reduced pressure. The toluene layer was washed with a common salt aqueous solution followed by drying with anhydrous sodium sulfate. Then, the sodium sulfate was removed from the mixture and the resultant mixture was evaporated to obtain a residue. Ethyl acetate was added to the residue and cooled with ice water to precipitate a crystal. The crystal was recovered by filtration and purified by silica gel column chromatography (eluent: toluene) and recrystallized from a mixture solvent (toluene/ethyl acetate). The resultant crystal was further purified by silica gel column chromatography (eluent: toluene/hexane=2/1) and recrytallized from a mixture solvent (toluene/hexane) to obtain 0.39 g of 2-octyl-5-[4-(4-decylphenyl)phenyl]indan (Yield: 41.3%). ##STR312##

1. temperatureheat-refluxed for 4 hours
2. customAfter the reaction
3. filtrationto followed by filtration under reduced pressure
4. washThe toluene layer was washed with a common salt aqueous solution
5. dry with materialby drying with anhydrous sodium sulfate
6. customThen, the sodium sulfate was removed from the mixture
7. customthe resultant mixture was evaporated
8. customto obtain a residue
9. customto precipitate a crystal
10. filtrationThe crystal was recovered by filtration
11. custompurified by silica gel column chromatography (eluent: toluene)
12. customrecrystallized from a mixture solvent (toluene/ethyl acetate)
13. customThe resultant crystal was further purified by silica gel column chromatography (eluent: toluene/hexane=2/1)