| 2-甲硫基-4-羟基-5-嘧啶甲酸乙酯的工艺优化 |
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| 引用本文： | 王海涛,王宏雁,杨亮茹,毛璞,屈凌波.2-甲硫基-4-羟基-5-嘧啶甲酸乙酯的工艺优化[J].应用化学,2015,32(4):412-415. |
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| 作者姓名： | 王海涛 王宏雁 杨亮茹 毛璞 屈凌波 |
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| 作者单位： | 河南工业大学化学化工学院 郑州 450000 |
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| 基金项目： | 国家自然科学基金资助项目(21172055) |
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| 摘 要： | 以S-甲基异硫脲半硫酸盐和乙氧基亚甲基丙二酸二乙酯为主要原料,乙醇为溶剂,合成出2-甲硫基-4-羟基-5-嘧啶甲酸乙酯,研究了2-甲硫基-4-羟基-5-嘧啶甲酸乙酯的工艺优化,考察了投料比、反应温度、反应时间等因素对产率的影响。 获得较好的反应条件:n(C2H6N2S·1/2H2SO4):n(C10H16O5):n(NaOH)=1.2:1:1.8,在室温下缓慢滴加NaOH溶液,搅拌反应6 h,酸化得白色固体产物,产率为81.1%。产物结构经熔点测定仪、1H NMR、ESI-MS、FT-IR等技术手段得到验证。
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| 关 键 词： | 甲硫基羟基嘧啶甲酸乙酯 工艺优化 嘧啶衍生物 |
| 收稿时间： | 2014-08-25 |
| 修稿时间： | 2014-11-14 |
Process Optimization of 4-Hydroxyl-2-(methylsulfanyl)-pyrimidine-5-carboxylic Acid Ethyl Ester Synthesis |
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| WANG Haitao,WANG Hongyan,YANG Liangru
,MAO Pu,QU Lingbo.Process Optimization of 4-Hydroxyl-2-(methylsulfanyl)-pyrimidine-5-carboxylic Acid Ethyl Ester Synthesis[J].Chinese Journal of Applied Chemistry,2015,32(4):412-415. |
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| Authors: | WANG Haitao WANG Hongyan YANG Liangru
MAO Pu QU Lingbo |
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| Institution: | School of Chemistry and Chemical Engineering,He'nan University of Technology,Zhengzhou 450000,China |
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| Abstract: | 4-Hydroxyl-2-(methylsulfanyl)-pyrimidine-5-carboxylic acid ethyl ester was synthesized from S-methylisothiourea hemisulfate salt and diethyl ethoxymethylenemalonate in ethanol. The feed ratio, reaction temperature, reaction time and other factors were optimized to improve the yield. The 81.1% yield of white solid product is obtained when the sodium hydroxide solution is dropwisely added into the reaction mixture in a molar ration of n(C2H6N2S·1/2H2SO4):n(C10H16O5):n(NaOH)=1.2:1:1.8 under stirring at room temperature for 6 h then with acid treatment. Its structure was characterized by melting point, 1H NMR, ESI-MS and FT-IR. |
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| Keywords: | hydroxyl-(methylsulfanyl)-pyrimidine-carboxylic acid ethyl ester optimization pyrimidine derivatives |
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