【摘要】：目的以鵝去氧膽酸為原料合成奧貝膽酸,以期得到更好的奧貝膽酸合成工藝。方法經(jīng)氧化、酯化、親電加成、催化加氫和水解還原共5步反應(yīng)得到奧貝膽酸(6α-乙基鵝去氧膽酸)新的合成工藝,總收率達(dá)38%。其結(jié)構(gòu)經(jīng)1H-NMR、MS分析測試技術(shù)確認(rèn)。結(jié)果通過考察各步反應(yīng)條件,得出最佳工藝條件:氧化反應(yīng)中,鵝去氧膽酸與N-溴代琥珀酰亞胺物質(zhì)的量比為1∶1.5;親電加成中,3α-羥基-7-酮-5β-膽烷酸-24-甲酯與三乙胺與叔丁基二甲基氯硅烷物質(zhì)的量比為1∶2∶2.2;還原反應(yīng)中,3α-羥基-6-亞乙基-7-酮-5β-膽烷酸-24-甲酯與硼氫化鈉物質(zhì)的量比為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 偽 -ethyl chenodeoxycholic acid (6 偽 -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 偽 -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 偽 -hydroxy-6-ethyl-7-keto-5 尾 -cholanoic acid-24 methyl ester to sodium borohydride is 1: 6.
【作者單位】： 南京理工大學(xué)化工學(xué)院;
【分類號】：R914.5

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