| 1-磺酸甲基四氮唑-5-硫醇双钠盐的合成 |
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| 引用本文： | 张玲,张岩,朱玉辐,薛运生,杨宜华,缑灵山,王丽莎,刘毅.1-磺酸甲基四氮唑-5-硫醇双钠盐的合成[J].精细石油化工,2011,28(6):20-23. |
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| 作者姓名： | 张玲 张岩 朱玉辐 薛运生 杨宜华 缑灵山 王丽莎 刘毅 |
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| 作者单位： | 1. 徐州医学院药学院,江苏徐州,221004
2. 徐州医学院附属医院神经外科,江苏徐州,221002 |
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| 基金项目： | 江苏高校优势学科建设工程资助项目，江苏省自然科学基金资助项目，江苏省高校自然科学基金资助项目，徐州医学院肿瘤生物治疗实验室资助项目，江苏省"青蓝工程"资助，江苏省高校科研成果产业化推进项目，徐州医学院第二批院长专项人才基金，徐州市科技计划指导项目，徐州市科技项目 |
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| 摘 要： | 以氨基甲磺酸为原料,经烷基化、环合、成盐等反应合成头孢尼西钠的重要中间体1-磺酸甲基四氮唑-5-硫醇双钠盐.将微波辐射技术应用到烷基化反应中,探讨了微波辐射功率、时间、溶剂对反应的影响,最佳反应条件为:以乙醇和水为溶剂,微波辐射功率250 W,辐射8 min,磺甲基二硫代氨基甲酸乙酯钾盐的收率84.0％；用乙醇钠成盐,...
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| 关 键 词： | 1-磺酸甲基四氮唑-5-硫醇双钠盐 头孢尼西钠 微波合成 中间体 |
SYNTHESIS OF 1-SULFOMETHYLTETRAZOLE-5-THIOL DISODIUM SALTS |
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| Zhang Ling,Zhang Yan,Zhu Yufu,Xue Yunsheng,Yang Yihua,Gou Lingshan,Wang Lisha,Liu Yi.SYNTHESIS OF 1-SULFOMETHYLTETRAZOLE-5-THIOL DISODIUM SALTS[J].Speciality Petrochemicals,2011,28(6):20-23. |
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| Authors: | Zhang Ling Zhang Yan Zhu Yufu Xue Yunsheng Yang Yihua Gou Lingshan Wang Lisha Liu Yi |
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| Abstract: | 1-Sulfomethyltetrazole-5-thiol disodium salts,a key intermediate of cefonicid sodium,was synthesized from aminomethanesulfonic acid,via alkylation under microwave irradiation,cyclization and salification reaction,with an overall yield of 68.1%(based on aminomethanesulfonic acid) and purity of 99.3%(HPLC).Effects of irradiation power,irradiation time and solvent on the alkylation reaction were discussed.The optimal conditions were obtained as follows: microwave irradiation power 250 W,irradiation time 8 min,water and ethanol as solvent,with 84.0% yield of ethyl sulfomethyldithiocarbamate potassium salt.Effects of salification reagent on the product yield,purity and structure were also studied.With sodium ethoxide as salification reagent,the yield of 1-sulfomethyltetrazole-5-thiol disodium salts was 88.3%.The structure of the aimed compound was confirmed by IR,1H NMR,MS and elemental analysis. |
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| Keywords: | 1-sulfomethyltetrazole-5-thiol disodium salts cefonicid sodium microwave synthesis intermediate |
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