2-乙酰基雌酚酮和2-乙酰基雌二醇-17β-乙酸酯的晶体和分子结构

The Crystal and Molecular Structure of 2-Acetyl-3-Hydroxyestra-l,3,5(10)-Trien- 17-one(3a) and 2-Aceryl-Estra-l,3,5(10)-Trien-3, 170-Diol 17-Acetate(3b)

雌甾化合物的晶体结构已有较多的研究,本文用X射线衍射法对2-乙酰基雌酚酮(Ⅰ)和2-乙酰基雌二醇-17β-乙酸酯(Ⅱ)二化合物的晶体和分子结构进行了研究。 1 实验 1.1 晶体培养 样品(Ⅰ)和(Ⅱ)按文献所述方法合成。在室温下将(Ⅰ)的吡啶溶液置于充满甲醇蒸气的密闭容器中,使溶液保持过饱和状态而逐渐长成浅黄色的透明晶体。将(Ⅱ)溶于乙酸乙酯中,经重结晶得无色的透明晶体。

In this paper, 2-Acetyl-3-hydroxyestra-1,3,5(10)-trien-17-one (3a) ( Ⅰ ) and 2-Acetyl-estra-1,3,5 (10)-trien-3, 17BB-diol 17-acetate (3b) ( Ⅱ ) were synthesized, and their single crystals have were grown. The crystal structures of compound ( Ⅰ ) and ( Ⅱ ) were determined on the Nicolet four-circle diffractometer. Both compounds ( Ⅰ ) and ( Ⅱ ) belong to orthogonal crystal system. Crys-tallographicdata. ( Ⅰ ) space group C2221, a=10. 4361(29) A, 6=11. 6299(36) A , c=29. 2196 (107) A. V = 3546. 41(1. 82) A3, Z = 8; (Ⅱ ) space group p212121, a=7. 2312(21) A , b = 12. 9008(50) A, c=20.6798(75) A, V=1929.16(75) A3 Z=4. The rough molecular structures were obtained by the direct method. Refinement was carried out by the full-matrix least-square. The structures were refined to final R1 =0. 0423 and RⅡ =0. 0368 for 1092 and 1625 observational reflections respectively. The results show that molecular inner-hydrogen bonds exist in both compounds ( Ⅰ ) and ( Ⅱ ). Ring A of both compounds is planar and ring B, C and D are semi-chair, chair and envelope forms, respectively.