TEMPO催化合成3α-羟基-7-酮-5β-胆烷酸的研究

Study of TEMPO Catalyst to Compound 3α-Hydroxy-7-Ketone-5β-Ursodeoxycholic Acid

建立了由TEMPO、NaClO和Na Br所组成的催化体系,考察了反应时间、温度、pH值、各物料之间的投料比对反应的影响程度。结果表明：鹅去氧胆酸、次氯酸钠、溴化钠的较佳投料摩尔比为1.0：1.2：0.1,次氯酸钠较佳p H值为9.2,反应时间控制在2h,温度控制在-5-0℃,总收率达到66.0%,具有工业化的应用价值。

This paper establishes the catalytic system composed by TEMPO, NaCIO and NaBr and investigates the influence degree of reaction time, temperature, pH value and weight ratio between each kind of material on the reaction. The results show that the better molar ratio of chenodeoxycholie acid, sodium hypochlorite and sodium bromide are 1.0：1.2：0.1, besides, the better pH value of sodium hypochlorite is 9.2, the reaction time is controlled in 2 h, the temperature is controlled in -5 - 0℃ and the total yields reached 66.0%, which has industrialized application value.