| 枸橼酸西地那非及关键中间体合成工艺的改进 |
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| 作者姓名： | 徐莉莉 汪海洋 孔意 姚庆强 |
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| 作者单位： | 1. 济南大学,山东省医学科学院医学与生命科学学院,山东 济南250022;山东省医学科学院药物研究所,山东 济南250062;章丘区人民医院,山东 济南250200;2. 济南大学,山东省医学科学院医学与生命科学学院,山东 济南250022;山东省医学科学院药物研究所,山东 济南250062;3. 济南明鑫制药股份有限公司,山东 济南,250216 |
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| 摘 要： | 目的 对枸橼酸西地那非及关键中间体西地那非合成工艺进行优化改进.方法 以邻乙氧基苯甲酰氯与4-氨基-1-甲基-3-正丙基-1H-吡唑-5-甲酰胺为起始物料,经缩合、环合、氯磺化、磺酰胺化、成盐等一系列反应,制备枸橼酸西地那非.结果 关键中间体西地那非纯度在99.5%以上,杂质D(《欧洲药典》)控制在0.3%以下,其他单杂控制在0.15%以下.结论 用精制后西地那非制备出枸橼酸西地那非,纯度在99.8%以上,总收率在45%以上.此工艺成本低,容易操作,且适合工业化生产.
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| 关 键 词： | 枸橼酸西地那非 关键中间体 杂质D 合成工艺 改进 |
The improvement of synthesis process for sildenafil citrate and its key intermediate |
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| Authors: | XU Lili WANG Haiyang KONG Yi and YAO Qingqiang |
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| Abstract: | Objective To optimize and improve the synthesis process for sildenafil citrate and its key intermediate sildenafil.Methods The sildenafil citrate was prepared from the raw materials of 2-ethoxybenzoyl chloride and 4-amino-1-methyl-3-n-propyl-5-pyrazolecarboxamide by the reactions of condensation,cyclization,chlorosulfonation,sulfonamide and salt.Results The purity of the key intermediate sildenafil was higher than 99.5%,impurity D(EP) was lower than 0.3% and the unspecified single impurity was lower than 0.15%.Conclusion The purity of the sildenafil citrate was above 99.8% and the total yield was 45%.The process was low cost,easy operate and suitable for industrialized production. |
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| Keywords: | Sildenafil citrate Key intermediate Impurity D Synthesis process Improvement |
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