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      降脂藥非諾貝特的工藝改進
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      作者單位:

      1.江蘇海洋大學 藥學院;2.江蘇德源藥業股份有限公司;3.江蘇海洋大學 環境與化學工程學院

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      中圖分類號:

      TQ460.6

      基金項目:

      國家自然科學基金青年基金項目(52103042);江蘇省蘇北科技專項(SZ-LYG202017);連云港市“花果山英才計劃”科技副總項目資助(2019.12);江蘇省大學生創新項目(SZ202111641640001)


      Improved synthesis of fenofibrate as the lipid-lowering drug
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      Affiliation:

      1.School of Pharmacy,Jiangsu Ocean University;2.Jiangsu Deyuan Pharmaceutical Co,Ltd;3.School of Environmental and Chemical Engineering,Jiangsu Ocean University

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        摘要:

        摘要:以對氯苯甲酰氯為原料,FeCl3催化苯甲醚和對氯苯甲酰氯發生Friedel-Crafts?;磻?-氯-4'-甲氧基二苯甲酮,繼而水解生成4-氯-4'-羥基二苯甲酮,4-氯-4'-羥基二苯甲酮再與丙酮、氯仿縮合得到非諾貝特酸;非諾貝特酸再和異丙醇酯化生成非諾貝特,進一步純化后制備非諾貝特晶體。采用MS、FTIR、X 單晶衍射、1HNMR和13CNMR對產物結構進行表征;并用X射線單晶衍射儀解析了非諾貝特晶體結構??疾炝送读狭?、反應溫度以及精制溶劑等因素對非諾貝特中間體及非諾貝特收率的影響。結果表明,合成4-氯-4'-甲氧基二苯甲酮的優化條件為:n(苯甲醚)∶n(三氯化鐵)∶n(對氯苯甲酰氯)=4.0∶0.0125∶1.0,145~155 ℃反應6 h;合成非諾貝特酸的優化條件為:n(氯仿)∶n(4-氯-4'-羥基二苯甲酮)=2.5∶1.0,析晶溫度為10 ℃,析晶溶劑為甲苯;合成非諾貝特的優化條件為:n(非諾貝特酸)∶n(異丙醇)∶n(濃硫酸)=1.0∶3.0∶2.0,用異丙醇精制得到非諾貝特晶體。非諾貝特的總收率可達56.17%(以對氯苯甲酰氯計),產物HPLC純度達99.93%。

        Abstract:

        Abstract: Using p-chlorobenzyl chloride as raw material, Friedel-Crafts acylation of anisole and p-chlorobenzoyl chloride was catalyzed by FeCl3, followed by hydrolysis to produce 4-chloro-4 '- hydroxybenzophenone, which reacted with acetone and chloroform by condensation to obtain fenofibrate acid. And then fenofibrate was synthesized by esterification with fenofibrate acid and isopropanol and further purification to prepare fenofibrate crystals. The structure of the product was characterized by MS, FTIR, X-ray diffraction, 1HNMR and 13CNMR. The crystal structure of fenofibrate was analyzed by X-ray crystal structure analysis. The effects of feed rate, reaction temperature and refining solvent on the yield were investigated. The optimum conditions for the synthesis of 4-chloro-4'- methoxy benzophenone are as follows: n(anisole):n(FeCl3):n(4-chlorobenzoyl chloride)=4.0:0.0125:1.0, acylation under 145~155 ℃ for 6h. The optimized conditions for synthesis of fenofibrate acid were as follows: n(CHCl3):n(4-chloro-4'-hydroxybenzophenone)=2.5:1.0, and crystallization with toluene at 10 ℃. The optimized conditions for synthesis of fenofibrate were as follows: n(fenofibrate acid):n(isopropyl alcohol):n(H2SO4)=1.0:3.0:2.0, purification with isopropyl alcohol to obtain crystals. The total yield and content of fenofibrate were 56.17% and 99.93%, respectively.

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      滿莉莉,李樹亮,楊漢躍,閆顯光,董淑波,張珍明.降脂藥非諾貝特的工藝改進[J].精細化工,2023,40(7):

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      歷史
      • 收稿日期:2022-09-27
      • 最后修改日期:2023-01-03
      • 錄用日期:2023-01-03
      • 在線發布日期: 2023-08-14
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