23-甲基胆-3β,5α,6β,20-四醇的合成

摘要

To synthesize a derivative of 3β,5α,6β-trihydroxypregn-20-one,3β,5α,6β-trihydroxy pregn-20-one was prepared from pregnenolone as raw materials through 30% H2 O2 oxidation in formic acid,the yield and melting point were found to be 19. 6 % and 256~258 ℃ respectively. 23-methylchol-3β,5α, 6β,20-tetraol was synthesized from 3β,5α,6β-trihydroxypregn-20-one and Isobutyl magnesium bromide through grignard reaction at room temperature in anhydrous THF in 5 h and then hydrolysing in 1 h by addition of 10 % sulfuric acid solution. The yield was 10. 6 %, and m. p. 180. 5 ~182. 0 ℃. The two compounds were corroborated structurally by IR and 1 H-NMR.%研究了3β,5α,6β-三羟基孕甾-20-酮衍生物的合成.以孕烯醇酮为原料在无水甲酸中以质量分数30%的过氧化氢( H2 O2)溶液氧化、甲醇中碱水解得3β,5α,6β-三羟基孕甾-20-酮,收率19．6%,m． p．256~258℃,再以3β,5α,6β-三羟基孕甾-20-酮与异丁基溴化镁在无水四氢呋喃中室温反应5 h,然后加入质量分数10%的硫酸继续反应约1 h,得23-甲基胆-3β,5α,6β,20-四醇,收率10．6%,m． p．180．5~182．0℃.经IR和1 H-NMR确证结构正确.