| 微波催化合成5,5-二甲基-2-重氮-1,3-环己二酮的探究 |
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| 引用本文： | 徐应淑,杨俊,徐小婷,袁清. 微波催化合成5,5-二甲基-2-重氮-1,3-环己二酮的探究[J]. 广东化工, 2014, 0(14): 33-34 |
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| 作者姓名： | 徐应淑 杨俊 徐小婷 袁清 |
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| 作者单位： | 遵义医学院药学院,贵州遵义563003 |
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| 基金项目： | 贵州省科技厅基金（黔科合J字2011[2083]号） |
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| 摘 要： | 目的探索在不同微波条件下,催化合成5,5-二甲基-2-重氮-1,3-环己二酮的最佳条件。方法在50 mL圆底烧瓶中加入双甲酮、乙腈、对甲苯磺酰叠氮和无水碳酸钾,在不同微波功率、反应时间和温度的条件下进行反应,通过TLC跟踪检测,柱色谱法、重结晶法等分离提纯产物。结果得到白色或类白色针状或块状晶体,并通过测定该晶体熔点,红外光谱(IR)、紫外光谱(UV)、核磁共振氢谱(1H NMR),核磁共振碳谱(13C NMR)等确证其结构。结论所合成的化合物与目标化合物一致。
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| 关 键 词： | 重氮环己酮 微波 合成 光谱解析 |
Microwave Catalytic Synthesis of 5,5-Dimethyl-2-Diazo 1,3-Cyclohexanedione |
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| Xu Yingshu,Yang Jun,Xu Xiaoting,Yuan Qing. Microwave Catalytic Synthesis of 5,5-Dimethyl-2-Diazo 1,3-Cyclohexanedione[J]. Guangdong Chemical Industry, 2014, 0(14): 33-34 |
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| Authors: | Xu Yingshu Yang Jun Xu Xiaoting Yuan Qing |
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| Affiliation: | (School of Pharmacy, zunyi Medical College, Zunyi 563003, China) |
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| Abstract: | Objective To explore the optimum conditions, catalytic synthesis of 5,5 -dimethyl-2 - diazo 1,3 - cyclohexanedione under different microwave conditions. Methods 50 mL round bottom flask was added dimedone, acetonitrile, p-toluenesulfonyl azide and anhydrous potassium carbonate and the reaction was carried out at different microwave power, reaction time and temperature. The reaction was purified by TLC, column chromatography, re-crystallization method for separating and purifying the product. Results Get white or similar white needle-like or lumps crystals, and its structure was confirmed by measuring the crystal melting point, infrared spectroscopy （IR）, ultraviolet spectroscopy （UV）, nuclear magnetic resonance spectroscopy （1H NMR）, carbon nuclear magnetic resonance spectroscopy （13C N MR）, etc. Conclusions： Spectrograms to ascertain the compound was consistent with the target one. |
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| Keywords: | diazo cyclohexanone microwave synthesis spectral analysis |
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