2,3α-环氧-3β-咪唑-5α-雄甾-17-酮的合成及其晶体结构

摘要

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-( lH-imidazol-l-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 monodinic system, space group P21 with a = 1.0615 mn, 6=0. 581 7 nm, c = 1.628 9 run,α = γ = 90°, 0 = 105.594°, R1=0.042 9, ωR2=0.114 3.%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-3-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 5nm,b=0.581 7nm,c=1.6289 nm,α=γ=90°,β=105.594°,R1 =0.0429,ωR2 =0.114 3.