L-2-methylbutyl-4-hydroxylbiphenyl-4′-carbonylate was synthesized from 4-hydroxylbiphenyl,4-hydroxyl-4′-cyanobiphenyl and chiral alcohol L-2-methylbutanol by three synthesis routes.The total yield was 35.6% by five-step method(etherification,F-C acylation,haloform-reaction,hydrolysis and esterification).The total yield was 50.7% by three-step method(F-C acylation,haloform-reaction and esterification).The yield by one step method was 64.4%.The structures were confirmed by ~1H NMR and IR.