N-(Benzyloxycarbonyl)-6-aminocaproic acid (I) is reacted with 1,8-octanediamine (II) to give amide (III). The protecting group can be removed either by hydrogenolysis or by gaseous HBr affording (IV), which is reduced with borane-methyl sulfide complex to yield N,N'-bis(6-aminohexyl)-1,8-octanediamine (V). Condensation of (V) with 2-methoxybenzaldehyde and subsequent reduction of the intermediate Schiff base gives methoctramine. However, methoctramine can be prepared more conveniently by transforming (IV) to (VI) followed by reduction of amide groups with borane.