反应详情

(S)-1-(3-pyridyl)ethanol (2.0 g) prepared in the above item (ii), 4-octyloxybiphenyl-4'-carboxylic acid (5.3 g), dicyclohexylcarbodiimide (5.7 g) and dimethylaminopyridine (0.2 g) were dissolved in methylene chloride (100 ml), followed by agitating the solution for 15 hours, thereafter filtering off insolubles, washing the filtrate with water, concentrating it and recrystallizing from a mixed solvent of heptane-toluene to obtain (S)-4-octyloxybiphenyl-4'-carboxylic acid-1-(3-pyridyl)ethyl ester (0.5 g). M.P.: 77.5-78.5° C. Specific angle of rotation [a]D25 =+95° (c=1.0, CHCl3). Further, the structure of this product was confirmed according to NMR spectra and the product accorded with the captioned compound.

1. filtrationfiltering off insolubles
2. washwashing the filtrate with water
3. concentrationconcentrating it
4. customrecrystallizing from a mixed solvent of heptane-toluene