| 一步法合成(R)-α-硫辛酸 |
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| 引用本文： | 狄延鑫,宋宝安.一步法合成(R)-α-硫辛酸[J].精细化工,2007,24(10):991-995. |
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| 作者姓名： | 狄延鑫 宋宝安 |
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| 作者单位： | 贵州大学,精细化工研究开发中心,教育部绿色农药与农业生物工程重点实验室,贵州,贵阳,550025 |
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| 基金项目： | 贵州省工业科技攻关项目 |
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| 摘 要： | 为提高(R)-α-硫辛酸(Ⅱ)合成收率,降低生产成本,以R体α-甲基苄胺拆分6,8-二氯辛酸得到的(R)-6,8-二氯辛酸(Ⅰ)为原料,在水相中采用一步法合成Ⅱ。讨论了摩尔比、反应温度、滴加时间等诸因素对产物收率及比旋光度的影响,获得了较优合成条件:拆分反应中,n(6,8-二氯辛酸)∶n〔(R)-α-甲基苄胺〕=1∶0.48,反应温度35℃,盐酸酸化;取代反应中,n(Ⅰ)∶n(二硫化钠)=1∶1.2,反应温度75℃,滴加时间3.0 h。在该优化条件下,Ⅱ的总收率为30.0%,并在该条件下,将6,8-二氯辛酸投料量扩大至600 g,Ⅰ投料量扩大至222.0 g,所得Ⅱ平均总收率可达34.3%。
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| 关 键 词： | (R)-α-硫辛酸 (R)-6 8-二氯辛酸 拆分 医药原料 |
| 文章编号： | 1003-5214（2007）10-0991-05 |
| 修稿时间： | 2007-02-14 |
One-step Process of (R)-α-Lipoic Acid Synthesis |
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| DI Yan-xin,SONG Bao-an.One-step Process of (R)-α-Lipoic Acid Synthesis[J].Fine Chemicals,2007,24(10):991-995. |
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| Authors: | DI Yan-xin SONG Bao-an |
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| Affiliation: | Key Laboratory of Green Pesticide and Agricultrual Bioengineering of Ministry of Education, Center for Research and Development of Fine Chemicals, Guizhou University, Guiyang 550025, Guizhou , China |
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| Abstract: | To increase the yield of(R)-α-lipoic acid(Ⅱ) and reduce its cost,an one-step synthesis of Ⅱ by using(R)-6,8-dichlorooctanoic acid(Ⅰ) as starting material was described.The synthesis steps involved chiral resolution of 6,8-dichlorooctanoic acid by(R)-α-phenylethylamine and substitution reaction in water phase.The optimized parameters were as follow.In the chiral resolution,n(6,8-dichlorooctanic acid)∶n((R)-α-phenylethylamine)=1∶0.48,and reaction temperature is 35 ℃;in the substitution reaction,n(Ⅰ)∶n(Na2S2)=1∶1.2,the reaction temperature is 75 ℃,and the dropping time keeps 3.0 h.Under the optimal conditions,the total yield of Ⅱ was 30.0%.When starting material 6,8-dichlorooctanic acid was expanded to 600 g and Ⅰ was increased to 222.0 g,the total yield of Ⅱ was up to 34.3%. |
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| Keywords: | (R)-α-lipoic acid (R)-6 8-dichlorooctanic acid chiral resolution drug materials |
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