From the root of Calotropis gigantea, six compounds were isolated: 12-O-benzoyllineolon (1), 12-O-benzoyldeacetylmetaplexigenin (2), calotropone (3), 2,3-dimethoxyphenol (4), 2,5- dimethoxyphenol (5), 2-formyl-5-hydroxymethylfuran (6). The chemical structure of these compounds were elucidated by their NMR spectra and comparison with references.