| 对羟基苯乙酸-N,N-二甲基甲酰氨基甲酰甲酯的合成工艺研究 |
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| 引用本文： | 肖志强,翟帆,麻纪斌,曲秦,舒泉湧.对羟基苯乙酸-N,N-二甲基甲酰氨基甲酰甲酯的合成工艺研究[J].应用化工,2014(12):2237-2238. |
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| 作者姓名： | 肖志强 翟帆 麻纪斌 曲秦 舒泉湧 |
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| 作者单位： | 陕西新药技术开发中心; |
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| 摘 要： | 采用N,N-二甲基-2-氯乙酰胺、4-羟基苯乙酸、三乙胺等为原料,于乙腈中反应,HPLC跟踪检测合成对羟基苯乙酸-N,N-二甲基甲酰氨基甲酰甲酯(简称化合物B)。结果表明,最佳合成工艺参数为:反应时间12 h,反应温度60℃,溶剂用量为2 200 m L,物料比为n(4-羟基苯乙酸)∶n(N,N-二甲基-2-氯乙酰胺)=1∶1.10。在最佳条件下,收率86%,纯度98%以上。
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| 关 键 词： | 对羟基苯乙酸-N N-二甲基甲酰氨基甲酰甲酯 甲磺酸卡莫司他 中间体 合成 |
study on synthesis process of p-hydroxyphenyl acetic acid-N,N-dimethylformamide,dimethyl carbamyl |
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| XIAO Zhi-qiang;ZHAI Fan;MA Ji-bin;QU Qin;SHU Quan-.study on synthesis process of p-hydroxyphenyl acetic acid-N,N-dimethylformamide,dimethyl carbamyl[J].Applied chemical industry,2014(12):2237-2238. |
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| Authors: | XIAO Zhi-qiang;ZHAI Fan;MA Ji-bin;QU Qin;SHU Quan- |
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| Affiliation: | XIAO Zhi-qiang;ZHAI Fan;MA Ji-bin;QU Qin;SHU Quan-yong;The New Drug Technology Development Center; |
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| Abstract: | Using N,N-dimethyl-2-chloro-acetamide,4-hydroxyphenyl acetic acid,triethylamine,etc. as raw materials,the reaction in acetonitrile,HPLC trace detection hydroxyphenyl acetic acid synthesis-N,N-dim-ethylformamide,carbamoyl ester（ compound B）. The result showed that the optimal synthesis parameters：reaction time 12 h,the reaction temperature is 60 ℃,the amount of solvent is 2 200 mL,material ratio of N（4-hydroxyphenyl acetic acid）：N（N,N-dimethyl-2-chloroacetamide）= 1：1. 10. Under optimal con-ditions the yield was 86%,with a purity of over 98%. |
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| Keywords: | p-hydroxyphenyl acetic acid-N N-dimethylformamide dimethyl carbamoyl camostat mesy-late intermediate synthesis |
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