沈阳化工大学学报
瀋暘化工大學學報
침양화공대학학보
JOURNAL OF SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
2015年
2期
128-129,139
,共3页
23-甲基胆-3β,5α,6β,20-四醇%孕烯醇酮%合成
23-甲基膽-3β,5α,6β,20-四醇%孕烯醇酮%閤成
23-갑기담-3β,5α,6β,20-사순%잉희순동%합성
23-methylchol-3β,5α,6β,20-tetraol%pregnenolone%synthesis
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.
研究瞭3β,5α,6β-三羥基孕甾-20-酮衍生物的閤成.以孕烯醇酮為原料在無水甲痠中以質量分數30%的過氧化氫( H2 O2)溶液氧化、甲醇中堿水解得3β,5α,6β-三羥基孕甾-20-酮,收率19．6%,m． p．256~258℃,再以3β,5α,6β-三羥基孕甾-20-酮與異丁基溴化鎂在無水四氫呋喃中室溫反應5 h,然後加入質量分數10%的硫痠繼續反應約1 h,得23-甲基膽-3β,5α,6β,20-四醇,收率10．6%,m． p．180．5~182．0℃.經IR和1 H-NMR確證結構正確.
연구료3β,5α,6β-삼간기잉치-20-동연생물적합성.이잉희순동위원료재무수갑산중이질량분수30%적과양화경( H2 O2)용액양화、갑순중감수해득3β,5α,6β-삼간기잉치-20-동,수솔19．6%,m． p．256~258℃,재이3β,5α,6β-삼간기잉치-20-동여이정기추화미재무수사경부남중실온반응5 h,연후가입질량분수10%적류산계속반응약1 h,득23-갑기담-3β,5α,6β,20-사순,수솔10．6%,m． p．180．5~182．0℃.경IR화1 H-NMR학증결구정학.
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.
