Phytochemical investigation of Metasequoia glyptostroboids leaves resulted in the isolation of ten compounds. The structures were determined to be isoquercitrin (1), quercitrin (2), myricitrin (3), amentoflavone (4), sciadopitysin (5), isoginkgetin (6), 2,3-dihydrosciadopitysin (7), 2,3-dihydroisoginkgetin (8), 3β-acetoxy-8(17),13E-labdadien-15-oic acid (9) and β-sitosterol (10) by spectroscopic analyses. Isoquercitrin (1) was isolated from this plant for the first time.