Studies in Synthetic Chemistry
ISSN / EISSN : 2332-7944 / 2332-7960
Published by: Hans Publishers (10.12677)
Total articles ≅ 58
Latest articles in this journal
Studies in Synthetic Chemistry, Volume 09, pp 1-7; https://doi.org/10.12677/ssc.2021.91001
β-羰基砜是一类重要的有机合成砌块，合成该类化合物一直是研究热点。本文以四丁基碘化铵为媒介，在电化学条件下实现烯醇硅醚与各种取代的磺酰肼发生自由基磺酰化反应，经自由基加成和氧化，在最优条件下以55%~76%的收率合成了8种具有不同取代基的β-羰基砜类化合物。采用核磁共振和质谱等手段对产物结构进行表征，并提出了可能的反应机理。 β-carbonyl sulfone is a kind of important organic synthesis block, and the synthesis of this kind of compounds has been a research hotspot. In this paper, β-carbonyl sulfones with different substi-tuents were synthesized by the free radical sulfonation of enol silyl ethers with various substituted sulfonyl hydrazides in the medium of tetrabutylammonium iodide under electrochemical conditions. Through radical addition and oxidation, eight β-carbonyl sulfones with different subs-tituents were synthesized in 55%~76% yield under the optimal conditions. The products were characterized by NMR and MS, and the possible reaction mechanism was proposed.
Studies in Synthetic Chemistry, Volume 8, pp 25-32; https://doi.org/10.12677/ssc.2020.81003
本文以L-脯氨酸衍生的手性硫脲为催化剂，对苯甲醛与二乙基锌的不对称1,2-加成烷基化反应进行了研究。我们发现在最优化的催化剂反应条件下，该反应可以以高收率和中等的对映选择性得到1-苯基-1-丙醇化合物。该催化体系具有高效、低成本、反应条件温和等特点，为合成手性芳基醇类化合物提供了一条有效、方便的路径。 In this paper, a series of L-proline derived chiral thioureas were designed and synthesized. Then the resulting catalysts were applied into the 1,2-addition reation of diethylzinc to benzaldehyde, which provided 1-phenylpropan-1-ol with good to excellent yields, albeit with moderate enatioselectivity. The catalytic system is featured with high efficiency, low cost as well as mild reaction conditions, and it was proved to be an effective and convenient route for the synthesis of chiral aromatic alcohols.
Studies in Synthetic Chemistry, Volume 8, pp 33-41; https://doi.org/10.12677/ssc.2020.81004
本文以一系列亚磷酸酯为催化剂，对催化芳香醛亚胺与丙烯酸甲酯的氮杂Baylis-Hillman反应进行了系统研究。经过对该反应的溶剂、反应温度、底物浓度、催化剂进行了筛选和优化，我们发现亚磷酸二乙酯和1,4-二氮杂二环[2.2.2]辛烷(DABCO)能有效催化该反应。最后对一系列底物进行测试，所有反应能以中等到良好的收率得到α-亚甲基β-磺酰胺基丙烯酸酯产物。 The aza-Bayllis-Hillman reactions of imines and methyl acrylate catalyzed by achiral phosphite were studied. The reaction conditions, such as solvent, temperature, concentration, catalysts, and substrates were screened. The target products of α-methylene--sulfonamido acrylates were obtained with 25% - 78% yield.
Studies in Synthetic Chemistry, Volume 8, pp 43-47; https://doi.org/10.12677/ssc.2020.82005
开发了一种通过类曼尼希反应制备3,3’-双(哌啶-1-甲基)八氢联萘酚简捷的一锅法合成方法。在溶剂甲醇中，使用廉价易得的哌啶盐酸盐替代管制品哌啶，以高达81.1%的收率得到3,3’-双(哌啶-1-甲基)八氢联萘酚。该法不仅反应条件温和，后处理操作简单，而且收率高。 A concise one-pot synthetic method was developed to prepare (S)-3,3’-bis(piperidin-1-ylmethyl)- octahydrobinaphthol (H8BINOL) by Mannich-type reaction. In the solvent methanol, (S)-3,3’-bis (piperidin-1-ylmethyl) octahydrobinaphthol was obtained in high yield of up to 81.1% using cheap and readily available piperidine hydrochloride to replace the controlled chemical piperidine.
Studies in Synthetic Chemistry, Volume 8, pp 48-53; https://doi.org/10.12677/ssc.2020.82006
以N-正丙基-1H-1,2,4-三唑-3,5-二胺为起始原料与苯甲醛反应合成化合物I；化合物1与3-甲氧基-2-甲基丙烯酸甲酯反应生成化合物II，化合物II脱去苯甲醛保护得到目标产物2-氨基-6-甲基-4-正丙基-1,2,4-三唑[1,5-a]并嘧啶-5-酮(化合物III)。考察催化剂、摩尔比、反应温度对反应的影响，考察苯甲醛的回收利用情况。结果表明：化合物I的最佳工艺条件为冰醋酸催化剂，回流反应，化合物II的最佳催化剂为甲醇钠，115℃反应；酸性条件下脱保护得到目标产物。在最佳工艺条件下，化合物I的收率为96%以上，化合物II的收率达到90%以上，化合物III的收率在95%以上。 Compound I was synthesized from N-propyl-1H-1,2,4-Triazole-3,5-diamine as the starting material with benzene formaldehyde; which was then reacted Methyl (E)-3-Methoxy-2-Methyl propenoate obtain compound II；finally, compound II was then deprotected to obtain target product 2-Amino-6-methyl-4-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-5-one (compound III). The reaction was optimized by studying the catalyst, molar ratio, reaction temperature, and the recovery of benzaldehyde was further considered. The results showed that the best process conditions of compound I were ice acetic acid catalyst, reflux reaction, compound II’s best catalyst was sodium methanol, 115˚C reaction, and the target product was obtained under acidic conditions. Under the best process conditions, the yield of compound I is more than 96%, the yield of compound II is more than 90%, and the yield of compound III is more than 95%.
Studies in Synthetic Chemistry, Volume 08, pp 61-66; https://doi.org/10.12677/ssc.2020.84008
抑制剂改性方法可以直接有效地解决沥青释放挥发性有机物(VOCs)的问题。单一种类添加剂的加入会不可避免地对沥青高低温性能产生影响，尤其吸附剂类和阻燃剂类添加剂会导致沥青的低温延伸性能劣化，且单一种类添加剂难以达到理想的抑烟效果。因此，往往将不同种类添加剂复配使用，期望在抑烟的同时不影响沥青的使用性能。本文综述了沥青VOCs的危害，介绍了沥青VOCs复合抑制剂的研究进展，并对沥青VOCs复合抑制剂研究的前景进行了展望。 The method of inhibitor modification can solve the problem of volatile organic compounds (VOCs) released from asphalt directly and effectively. The addition of a single kind of additives will inevitably affect the high and low-temperature performance of asphalt, especially the adsorbent and flame retardant additives will lead to the deterioration of asphalt low-temperature elongation performance, and it is difficult to achieve the ideal smoke suppression effect. Therefore, different kinds of additives are often used together to suppress smoke without affecting the performance of asphalt. This paper summarizes the harm of asphalt VOCs, introduces the research progress of asphalt VOCs composite inhibitors, and prospects the research prospects of asphalt VOCs composite inhibitors.
Studies in Synthetic Chemistry, Volume 8, pp 16-24; https://doi.org/10.12677/ssc.2020.81002
光开光在很多光化学和光物理应用中起到非常重要的作用。本论文中，我们通过将BiCl3，4,4’-联吡啶，甲醇和浓盐酸混合，采用溶剂热方法制备了一例铋基光致变色无机–有机杂化材料，并对其光电导和光致发光调制性能进行了研究。光照前后，电导率由0.43 × 10−5 S·cm−1 减小到0.21 × 10−5 S·cm−1 ，并且获得了高达4次的循环稳定性，同时，光致变色过程实现了高达8倍的发光对比度。 Photoswitchable properties are very important in many photochemical and photophysical applications. In this work, a Bismuth-based photochromic inorganic-organic hybrid was prepared by solvothermal reaction with the mixture of BiCl3, 4,4’-bipyridine, CH3OH and concentrated HCl. The photoconduction and photoluminescence switchable properties have been studied. In the photochromic process, the electrical conductivity was dropped from 0.43 × 10−5 S·cm−1 to 0.21 × 10−5 S·cm−1 , with the stability of 4 cycles, and the process reached a luminescence contrast up to 8 times.
Studies in Synthetic Chemistry, Volume 8, pp 1-15; https://doi.org/10.12677/ssc.2020.81001
研究了六种不同β-二酮类化合物或芳香羧酸类化合物作为第一配体，在水浴法下对三元铕配合物合成的影响，分别用紫外可见分光光谱法、FT-IR、ICP、分子荧光光谱对三元配合物结构进行表征，计算产物纯度，分析发光性能，比较产率。并从合成方法和条件两方面对Eu(TTA)3(TPPO)2进行工艺优化。结果表明：Eu(TTA)3(TPPO)2是其中最佳稀土铕配合物；工艺优化方面，得到微波辅助法的效率高于水浴法和超声法的结论；较优工艺条件：微波辐射反应时间20 min，微波功率200 W，料液比1:15，优化条件下的产收为68.63%。The effect of six different β-diketones or aromatic carboxylic acids as the first ligands on the synthesis of Ternary Europium Complexes by using waterbath was investigated. The structures of Ternary Europium Complexes were characterized by UV-vis spectrometry, FT-IR, ICP and molecular fluorescence spectra respectively to calculate product purity. The luminescent properties were analyzed and the yields were compared. The process of Eu(TTA)3(TPPO)2 was optimized from the aspects of synthesis method and conditions. The results show that Eu(TTA)3(TPPO)2 was the best rare earth europium complex. In terms of process optimization, the efficiency of microwave-assisted method was higher than that of water bath method and ultrasonic method. The optimal process conditions were as follows: microwave irradiation reaction time 20 min, microwave power 200 W, material solid-liquid ratio 1:15. Under the optimized conditions, the yield was 68.63%.
Studies in Synthetic Chemistry, Volume 8, pp 55-60; https://doi.org/10.12677/ssc.2020.83007
Studies in Synthetic Chemistry, Volume 7, pp 7-10; https://doi.org/10.12677/ssc.2019.72002
以1-苄基哌啶酮为原料，先与苯胺和三甲基硅氰发生Strecker反应得到化合物2，再经过酰胺化、甲酯化、N-丙酰化等三步反应，以26%的总收率合成了1-苄基哌啶酮衍生物，产物结构经1H NMR、13C NMR和HRMS表征。该方法具有绿色、简便的特点。 The compound 2 was prepared by the Strecker reaction of 1-benzylpiperidone with aniline and trimethylsilyl cyanide. Then 1-benzylpiperidone derivatives were synthesized in 26% overall yield by amidation, methyl esterification and N-propionylation. The structure of the product was characterized by 1H NMR, 13C NMR and HRMS. The method is green and simple.