奥贝胆酸的合成工艺

发布时间：2018-10-26 10:07

【摘要】：目的以鹅去氧胆酸为原料合成奥贝胆酸,以期得到更好的奥贝胆酸合成工艺。方法经氧化、酯化、亲电加成、催化加氢和水解还原共5步反应得到奥贝胆酸(6α-乙基鹅去氧胆酸)新的合成工艺,总收率达38%。其结构经1H-NMR、MS分析测试技术确认。结果通过考察各步反应条件,得出最佳工艺条件:氧化反应中,鹅去氧胆酸与N-溴代琥珀酰亚胺物质的量比为1∶1.5;亲电加成中,3α-羟基-7-酮-5β-胆烷酸-24-甲酯与三乙胺与叔丁基二甲基氯硅烷物质的量比为1∶2∶2.2;还原反应中,3α-羟基-6-亚乙基-7-酮-5β-胆烷酸-24-甲酯与硼氢化钠物质的量比为1∶6。
[Abstract]:Objective to synthesize Obercholic acid from chenodeoxycholic acid in order to obtain a better synthetic process. Methods A new synthetic process of 6 伪 -ethyl chenodeoxycholic acid (6 伪 -ethyl chenodeoxycholic acid) was obtained by oxidation, esterification, electrophilic addition, catalytic hydrogenation and hydrolysis and reduction. The overall yield was 38%. Its structure was confirmed by 1H-NMRMS analysis and test technique. Results the optimum reaction conditions were as follows: the ratio of chenodeoxycholic acid to N-bromosuccinimide was 1: 1.5; In the electrophilic addition, the molar ratio of 3 伪 -hydroxy-7-keto-5 尾 -cholanoic acid-24 methyl ester and triethylamine to tert-Ding Ji dimethyl chlorosilane is 1: 2: 2.2; In the reduction reaction, the ratio of 3 伪 -hydroxy-6-ethyl-7-keto-5 尾 -cholanoic acid-24 methyl ester to sodium borohydride is 1: 6.
【作者单位】：南京理工大学化工学院;
【分类号】：R914.5

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