2,3α-环氧-3β-咪唑-5α-雄甾-17-酮的合成及其晶体结构

Synthesis and Crystal Structure of 2,3α-Epoxy-3β-(1H-imidazol-1-yl)-5α-androstan-17-one

5α-表雄甾经Jones氧化与溴化反应制得2α-溴-5α-雄甾-3,17-二酮(3);3与咪唑在DMF/K2CO3体系中反应成功地合成了2,3α-环氧-3β-咪唑-5α-雄甾-17-酮(4),其结构经1H NMR,13C NMR,IR,MS和XRD表征。4属单斜晶系,空间群P21,晶胞参数a=1.061 5 nm,b=0.581 7 nm,c=1.628 9 nm,α=γ=90°,β=105.594°,R1=0.042 9,ωR2=0.114 3。

2α-Bromine-5α-androstan-3,17-dione（3） was prepared from epiandrosterone by a two-step reaction of Jones oxidation and bromination.2,3α-Epoxy-3β-（1H-imidazol-1-yl）-5α-androstan-17-one（4） was synthesized by the reaction of 3 with imidazol in DMF/K2CO3 system.The structure was characterized by 1H NMR,13C NMR,IR,MS and XRD.4 belongs to monoclinic system,space group P21 with a=1.061 5 nm,b=0.581 7 nm,c=1.628 9 nm,α=γ= 90°,β=105.594°,R1=0.042 9,ωR2=0.114 3.