A new triterpenoid glycoside, heterobetulinic acid 3-O - D-glucopyranosyl(1→2) - D-xylopyranoside (1), together with a new phenylacrylic acid derivative, 3S,4-dihydroxyl-2-methylene-but-1-enyl caffeate (2), were isolated from the roots of Ilex pubescens. Their structures were elucidated by HR-ESI-MS, 1-D and 2-D NMR analyses and chemical methods. In addition, the absolute configuration of 2 was established by the application of a modified Mosher's method.