Synthesis and purification of13C labelled xanthine derivatives

3-[Methyl- 13 C]xanthine, 7-[Methyl- 13 C]xanthine, 1,3-[Dimethyl- 13 C 2 ]xanthine (theophylline-1,3 [ 13 CH 3 ] 2 ), 1,7-[Dimethyl- 13 C 2 ]xanthine (paraxanthine-1,7-[ 13 CH 3 ] 2 ), and 3,7-[Dimethyl l3 C 2 ]xanthine (theobromine-3,7-[ 13 CH 3 ] 2 ) were synthesized by nucleophilic substitution reaction (SN 2 ) from xanthine (X) and iodomethane-[ 13 C]. The 3-isobutylparaxanthine-7-[ 13 CH 3 ] was prepared from 3-isobutyl-1-methylxanthine (IBMX). The compounds were purified by reverse phase semipreparative liquid chromatography and their chemical structure and purity verified by GC-MS.

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