The reductive cleavage of benzaldehyde acetals and acetophenone ketals with the air- stable crystalline 9-borabicyclo [3.3. 1] nonane dimer provides monobenzylated ether derivatives of diols and 1, 2-oxygen-transposed β-phenethyl alcohols, respectively. The boron moiety is effectively recovered through simple procedures which involve convenient air-stable reagents and boron byproducts. The process is particularly selective for 1, 3- ...