反应详情

First, 8 g of 2,3-difluoro-4'-(11-hydroxyundecyl)oxybiphenyl and 100 ml of carbon tetrachloride were placed in a 200 ml flask. A solution in which 2.3 g of phosphorus tribromide was dissolved in 50 ml of carbon tetrachloride was added dropwise to the reaction mixture under ice water cooling, and the resultant reaction mixture was stirred at room temperature for 3 hours and under reflux for 2 hours. The reaction mixture was poured into water, and an organic layer was extracted with ether. The ether layer was washed with water and dried over anhydrous sodium sulfate. Thereafter, the solvent was distilled away. The residue was purified by silica gel column chromatography (eluent: toluene/hexane=1/9) and recrystallized from hexane to obtain 4.5 g of 2,3-difluoro-4'-(11-bromoundecyl)oxybiphenyl (Y: 47.8%). The compound thus obtained had a purity of 95.3% by GC.

1. additionwas added dropwise to the reaction mixture under ice water cooling
2. customthe resultant reaction mixture
3. temperatureunder reflux for 2 hours
4. extractionan organic layer was extracted with ether
5. washThe ether layer was washed with water
6. dry with materialdried over anhydrous sodium sulfate
7. distillationThereafter, the solvent was distilled away
8. customThe residue was purified by silica gel column chromatography (eluent: toluene/hexane=1/9)
9. customrecrystallized from hexane