Selective oxidation of geranyl acetate (I) to the unsaturated aldehyde (II) was achieved by means of a two-step procedure with SeO2 and tert-butyl hydroperoxide, followed by treatment with MnO2. Reductive amination of aldehyde (II) with aniline using NaBH(OAc)3 furnished amine (III). After acetate ester hydrolysis in (III) employing K2CO3 in MeOH, the resulting allylic alcohol (IV) was converted to chloride (V) by treatment with triphenylphosphine dichloride. Finally, displacement of the chloride group of (V) with tris(tetra-n-butylammonium)hydrogenpyrophosphate provided the target pyrophosphate ester.