Resolution of 2-(3-indolyl)propionic acid was achieved via biocatalytic hydrolysis of its chloroethyl ester. Of the enzymes tested, Mucor javanicus lipase (R selectivity) and alpha-chymotrypsin (S selectivity) had high reactivity and enantioselectivity (E value > 50). Neither enzyme showed enantioselectivity (E value = 1) for 2-phenylpropionic acid.