Abstract: 11α-Methoxy-estradiol (12) was synthesized according to the method reported by Pierdet et al, with improvement in process. In addition to 11α-hydroxy-estradiol (11), 11β-hydroxy-estradiol (13), 11β-methoxy-estradiol (14) and 11α-methoxy-9β-estradiol (15) were synthesized from the same intermediate (3). The structures of synthetic products and key-intermediates were proved by ¹H-NMR, mass spectroscopy and elemental analysis. The estrogenic activity, of compounds (11), (12), (13), (14) and (15) was reported.