第 50 卷第 5 期 |  | Vol. 50 No. 5 | 2020 年 10 月 | Oct 2020 |
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所屬欄目:功能材料
二亞芐叉山梨醇合成新工藝研究 |
吳恩慧,張 燕,許蕓晗,王海蝶,李金洋,管西棟*
(山東第一醫科大學(xué)(山東省醫學(xué)科學(xué)院) 藥學(xué)院,山東 泰安 271016) |
摘 要:以山梨醇、苯甲醛為原料,在催化劑、助催化劑、脫水劑作用下,于常溫反應合成了二亞芐叉山梨醇(DBS)。采用紅外和核磁確認了DBS結構,考察了反應物配比、催化劑、助溶劑、助催化劑、吸水劑、反應時(shí)間和溫度等因素對產(chǎn)品收率的影響。結果表明:n(山梨醇)∶n(苯甲醛)=1.0∶2.0,以濃硫酸、對甲苯磺酸和磷鎢酸為催化劑,在二甲基亞砜和甲醇中室溫反應3 h時(shí),產(chǎn)品收率為95.9%,純度98.2%。 |
關(guān)鍵詞:二亞芐叉山梨醇;成核劑;催化劑;脫水劑;工藝優(yōu)化 |
中圖分類(lèi)號:TQ630 文獻標識碼:A 文章編號:1009-9212(2020)05-0057-04 |
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A Novel Synthesis Process of Dibenzylidene Sorbitol |
WU En-hui, ZHANG Yan, XU Yun-han, WANG Hai-die, LI Jin-yang, GUAN Xi-dong*
(School of Pharmaceutical Sciences, Shandong First Medical University&Shandong Academy of Medical Scicenes, Taian 271016, China) |
Abstract:Taking sorbitol and benzaldehyde as raw materials with the aid of catalysts, co-catalysts, and dehydrating agents, dibenzylidene sorbitol (DBS) was synthesized at room temperature. The structure of DBS was confirmed by IR and NMR, and the influence of factors including reactant ratio, catalyst, cosolvent, cocatalyst, water absorbent, reaction time and temperature on the product yield was investigated. The results showed that: n(sorbitol)∶ n(benzaldehyde)=1.0∶2.0, using concentrated sulfuric acid, p-toluenesulfonic acid and phosphotungstic acid as catalysts, reacting in dimethyl sulfoxide and methanol at room temperature for 3 h, the product yield was 95.9% with a purity of 98.2%. |
Key words:DBS; nucleating agent; catalyst;dehydrating agent; process optimization |
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基金項目:國家級大學(xué)生創(chuàng )新創(chuàng )業(yè)訓練計劃(201910439002),泰安市科技發(fā)展計劃引導項目(2017GX0067)。
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作者簡(jiǎn)介:吳恩慧(1998—),女,山東煙臺人,研究方向:有機合成與精細化工中間體合成(E-mail:485936232@qq.com)。
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聯(lián) 系 人:管西棟,實(shí)驗師,研究方向:有機合成與精細化工中間體合成(E-mail:xdguan@sdfmu.edu.cn)。
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收稿日期:2020-09-25
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