| 第 45 卷第 5 期 |  | Vol. 45 No. 5 | | 2015 年 10 月 | Oct 2015 |
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所屬欄目：醫藥及中間體
手性拆分劑一水合-L-二苯甲酰酒石酸的合成工藝研究 |
| 唐子涵1，周 銀2，徐 帥2，廖曉云1
（1. 長(cháng)沙市明德中學(xué)，湖南 長(cháng)沙 410006；2. 中南大學(xué) 化學(xué)化工學(xué)院，湖南 長(cháng)沙 410083） |
| 摘 要：以L(fǎng)-酒石酸、苯甲酰氯為起始原料，甲苯為溶劑，經(jīng)過(guò)酯化、酐化和水解2步反應得到手性拆分劑一水合-L-苯甲酰酒石酸，并優(yōu)化了工藝條件。結果表明，在n（L-酒石酸）∶n（苯甲酰氯）=1∶3.1、反應溫度為120~125℃、反應時(shí)間3.5 h及酸酐水解體系為甲苯／水、n（酸酐）∶n（水）=1∶4、反應溫度為100~105℃、水解時(shí)間3 h的反應條件下，目標化合物的總收率達84.1%，純度大于99.5%。該方法反應收率高，后處理簡(jiǎn)便，污染少，工藝條件易于控制，適合工業(yè)生產(chǎn)。 |
| 關(guān)鍵詞：手性拆分劑；L-酒石酸；L-二苯甲酰酒石酸；苯酰氯 |
| 中圖分類(lèi)號：O625 文獻標識碼：A 文章編號：1009-9212（2015）05-0034-04 |
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| Practical Syntheses of L-Dibenzoyltartaric Acid Monohydrate for Chiral Separation Agent |
| TANG Zi-han1, ZHOU Yin2, XU Shuai2, LIAO Xiao-yun1
(1. Mingde Middle School, Changsha 410006, China; 2. School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China) |
| Abstract：Using L-tartaric acid and benzoyl chloride as starting materials and toluene as the solvent, L-dibenzoyltartaric acid monohydrate was synthesized via esterification, anhydridization and hydrolysis. The influential factors on the reaction yield were evaluated. The optimum reaction conditions were obtained as follows: n(L-tartaric acid):n(benzoyl chloride)=1:3.1, reaction temperature 120~125℃, reaction time 3.5 h; in toluene-water hydrolysis process, n(L-dibenzoyltartaric anhydride):n(water)=1:4, reaction temperature 100~105℃, hydrolysis time 3 h. The target product was synthesized in high yield of 84.1% with high purity of 99.5%. The process has the advantages of high yield, simple operation, low pollution and easy-control process condition, therefore, this method have good prospect in industrial application. |
| Key words：chiral resolving agents; L-tartaric acid; L-dibenzoyltartaric acid; benzoyl chloride |
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作者簡(jiǎn)介：唐子涵（1997-），男，湖南長(cháng)沙人，主要從事藥物研究（E-mail：hongwai2012@163.com）。
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收稿日期： 2015-08-2
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