The thin layer chromatography on basic alumina of activity III(160-180 mesh) without binder has been applied to the separation of caffeine, theobromine, and theophyllene.With n-butanol: isoamyl alcohol : hydrochloric acid: water (8:2:1:20) as developing agents, the R_f values found were 0.924, 0.581, and 0.0 for caffeine,theobromine, and theophylline respectively. The angle of inclination employed for development wa 15-20°.