反应详情

First, 1.7 g of lithium borohydride and 20 ml of tetrahydrofuran were placed in a 100 ml flask. Then, 60 ml of tetrahydrofuran solution in which 4 g of 2,3-difluoro-4'-[12,12-bis(ethoxycarbonyl)dodecyl]oxybiphenyl was dissolved was added dropwise to the reaction mixture, and the resultant reaction mixture was stirred under reflux for 18 hours. The reaction mixture was poured into cold diluted hydrochloric acid, 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: ethyl acetate/toluene=8/2) and recrystallized from acetone to obtain 2.4 g of 2,3-difluoro-4'-[12,12-bis(hydroxymethyl)dodecyl]oxybiphenyl (Y: 71.6%). The compound thus obtained had a purity of 99.6% by HPLC.

1. additionwas added dropwise to the reaction mixture
2. customthe resultant reaction mixture
3. temperatureunder reflux for 18 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: ethyl acetate/toluene=8/2)
9. customrecrystallized from acetone