The transacetalization of 2-alkoxy-4-benzylidenetetrahydrofurans with alcohols proceeds smoothly with the aid of Fe(ClO4)3 catalyst. The catalyst reactivity is ordered as Fe(ClO4)3 > Zn(ClO4)2 > Mg(ClO4)2. The present transacetalization provides an entry for various 2-alkoxytetrahydrofurans, which have potential as anticancer agents.