共查询到19条相似文献,搜索用时 93 毫秒
1.
通过Cu(I)催化有机叠氮化物和端基炔之间的1,3-偶极Huisgen环加成反应,又称“点击化学”, 可快速、高效合成专一的1,4-二取代-1,2,3-三唑产物. 为得到含有末端炔的喹啉酮衍生物,以7,8-二氢-2,5(1H,6H)-二酮(1)为原料,通过烷基化反应将端基炔引入到化合物1中,合成了1-(2-炔丙基)-7,8-二氢喹啉-2,5(1H, 6H) 二酮(3),并利用重结晶和硅胶柱分离两种化学手段,得到了该化合物的两种构型异构体. 采用DEPT、1H NMR、13C NMR、1H-1H COSY、NOESY、HMQC多种NMR实验测试分析方法,对该化合物的构型异构体进行了验证和区分,并分别对其1H NMR和13C NMR谱的信号进行了归属. 相似文献
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以(2R,5S)-2,5-二甲基哌嗪为原料,经过成盐,单取代反应,用D-酉石酸对光学异构体的手性拆分,用氢氧化钠游离,最终合成(2R,5S)-N-间氟苄基-2,5-二甲基哌嗪,反应总收率为83%.该物质的合成未见文献报道,目标化合物用1H NMR,IR进行结构表征. 相似文献
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软骨凹顶藻Laurencia Cartilaginea 甾醇成分的研究 总被引:2,自引:0,他引:2
从中国南海软骨凹顶藻乙醇浸提物的乙酸乙酯相中 ,首次分离得到一种环二氧麦角甾醇 :5α,8α-环二氧麦角甾 - 6 ,2 2 -二烯 - 3β-醇 (1)。通过 GC- MS方法检测到了其他 5种甾醇化合物 :5 ,8-环二氧麦角甾 - 1,6 ,2 2 -三烯 - 3-醇 (2 ) ,麦角甾 - 6 ,2 2 -二烯 - 5 ,8-二羟基 - 3-酮 (3) ,豆甾 - 6 ,2 2 -二烯 - 5 ,8-二羟基 - 3-酮 (4) ,麦角甾 -5 ,7,9(11) ,2 2 -四烯 - 3-醇 (5 )以及豆甾 - 5 ,7,2 2 -三烯 - 3-醇 (6 ) 相似文献
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杨秀丽 《光谱学与光谱分析》1981,(5)
近年来,萃取原子吸收法测定微量金应用较普遍,但一般多采用盐酸介质以卤化金络阴离子形式进行萃取,因而大量铁严重干扰测定。此外据文献介绍,用高分子胺萃取金大致有:三辛胺二异丁基酮,含有季胺盐的二丁异丁基酮及三辛胺-氯仿等,这些方法虽快速, 相似文献
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以“一锅煮”方法合成了奈非那韦中间体-(3S,4aS,8aS)-2-((2R,3R)-3-氨基-2-羟基-4-(苯硫)丁基)-N-tert-丁基-十氢异喹啉-3-羧酰胺(Ⅶ),并以活泼酯新方法连接中间体Ⅶ得到了奈非那韦(Ⅸ)。在不同浓度和温度氢氧化钾的催化下,环合氯醇化合物(2R,3S)-4-氯-3-羟基-1-苯基硫丁基-2-氨基甲酸苄酯(Ⅲ),然后与(3S,4aS,8aS)-N-叔丁基-十氢异喹啉-3-羧酰胺(Ⅴ)反应,再脱去苄氧羰基保护基得中间体Ⅶ,收率89.0%。以2-甲基-3-乙酰氧基苯甲酸琥珀酰亚胺酯(Ⅱ)连接Ⅶ,再以浓氨水脱去乙酰基得奈非那韦(Ⅸ),收率86.0%。讨论了奈非那韦的红外光谱特征吸收峰所对应的官能团的振动形式,以MALDI-TOF MS(基质辅助激光解吸电离飞行时间质谱)得到了其分子离子及准分子离子峰, 利用一维(1HNMR,13C NMR)和DEPT (不失真极化转移增强谱)及HMBC(1H检测的异核多键相关谱)、HSQC(1H检测的异核单量子相干谱)、DQF-COSY(双量子过滤相干谱)等二维核磁共振波谱手段对奈非那韦的分子结构进行了表征, 并对其核磁谱线进行了归属分析。这对奈非那韦的结构鉴定及质量控制均有重要的参考价值。 相似文献
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1,3,4,6-tetramethylpiperazine-2,5-dione was synthesized, and the crystal structure was characterized by single-crystal X-ray diffraction method, vibrational spectral measurements were obtained by Fourier transform infrared spectroscopy and Fourier transform Raman spectroscopy. The measurements agree well with the calculated geometrical structure and harmonic vibrational wavenumbers (usingab initio and density functional theory Becke’s three parameters hybrid method with the Lee, Yang, and Parr non-local functions methods with 6-311G and 6-311G** basis sets). 相似文献
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Investigations of the inhibition of copper corrosion in nitric acid solutions by ketene dithioacetal derivatives 总被引:1,自引:0,他引:1
Ketene dithioacetal derivatives, namely 3-[bis(methylthio)methylene] pentane-2,4-dione (1), 3-(1,3-dithian-2-ylidene) pentane-2,4-dione (2) and 3-(1,3-dithiolan-2-ylidene) pentane-2,4-dione (3) were synthesized and their respective capacity to inhibit copper corrosion in 3 M HNO3 was investigated by means of weight loss, potentiodynamic polarization, scanning electron microscopy (SEM) and energy dispersive X-ray fluorescence (XRF). The obtained results indicate that the addition of these compounds significantly decreases the corrosion rate. Potentiodynamic polarization studies clearly showed that the inhibition efficiency increases with increasing concentration of the investigated compounds at a fixed temperature, but decreases with increasing temperature. These results on the whole showed that the studied substances are good cathodic inhibitors for copper corrosion in nitric acid medium. SEM and energy dispersive X-ray (EDAX) examination of the copper surface revealed that these compounds prevented copper from corrosion by adsorption on its surface to form a protective film, which acts as a barrier to aggressive agents. The presence of these organic compounds adsorbed on the electrode surface was confirmed by XRF investigations. 相似文献
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Melek Pamuk Algi Zahide Oztas Seha Tirkeş Atilla Cihaner Fatih Algi 《Journal of fluorescence》2017,27(2):509-519
Two chemiluminescent compounds containing 2,5-di(thien-2-yl)pyrrole and pyridazine units, namely 5,7-di(thiophen-2-yl)-2,3-dihydro-1H-pyrrolo[3,4-d]pyridazine-1,4(6H)-dione (5) and 6-phenyl-5,7-di(thiophen-2-yl)-2,3-dihydro-1H-pyrrolo[3,4-d]pyridazine-1,4(6H)-dione (6), were successfully synthesized and electrochemically polymerized. The compounds have chemiluminescent properties and glow in the presence of hydrogen peroxide in basic medium. The intensity of the glow can be increased dramatically by using Fe3+ ions, hemin (1.0 ppm) or blood samples (1.0 ppm) as catalyst. The compounds 5 and 6 have one well-defined irreversible oxidation peak at 1.08 V and 1.33 V vs Ag/AgCl, respectively. Electrochemical polymerization of both 5 and 6 were carried out successfully by repeating potential scanning in the presence of BF3. Et2O in an electrolyte solution of 0.1 M LiClO4 dissolved in acetonitrile. The electronic band gaps (Eg) of the polymers P5 and P6 were found to be 2.02 eV and 2.16 eV, respectively. On the other hand, the corresponding polymers are electroactive and exhibited electrochromic features. 相似文献
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V. Pashynska O. Boryak M. V. Kosevich S. Stepanian L. Adamowicz 《The European Physical Journal D - Atomic, Molecular, Optical and Plasma Physics》2010,58(3):287-296
A model study of the interaction between biologically active bisquaternary
ammonium salts and their molecular targets in living systems is urgently
needed to elucidate the molecular mechanisms involved in the interactions
between these compounds. To address this need a combined
experimental-computational study of the interaction of two
tetramethylammonium cations (modeling two quaternary groups) with the
chlorine anion and with the deprotonated 2,5-dihydroxybenzoic acid (modeling
a carboxylic group and an aromatic ring of side radicals of proteins) has
been performed. Fast atom bombardment mass spectrometry method and
DFT/B3LYP/6-31++G** and MP2/6-31++G** calculations have been employed in the
study. Stable noncovalent complexes with different ratios of the
tetramethylammonium cations and chlorine anions or deprotonated
2,5-dihydroxybenzoic acid anions were registered in the mass spectra of
tetramethylammonium chloride and 2,5-dihydroxybenzoic acid mixture. This
finding shows that the organic and inorganic anions compete to bind
tetramethylammonium in the studied system. The theoretically determined
stabilities of the noncovalent complexes were compared with the relative
stabilities evaluated from the mass spectrometric measurements. The results
of the study allow us to elucidate the competing interactions that exist
between quaternary groups with inorganic counterions or with active groups
of molecular protein targets. 相似文献
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Multicomponent reactions involving azines (phenanthridine or isoquinoline) and dimethyl acetylenedicarboxylate were undertaken in the presence of heterocyclic NH compounds (indole, 2-methyl indole, 3-methyl indole, carbazole and 3,6-dibromocarbazole) or 1,3-dicarbonyl compounds such as N,N'-dimethylbarbituric acid, 1,3-diethyl-2-thiobarbituric acid, acetylacetone, 1,3-diphenyl-1,3-propandione and cyclopentan-1,3-dione to generate enaminoesters in good yields. 相似文献
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Poly (ADP-ribose) polymerase (PARP-1) is a well-established nuclear protein with prominent role in signaling and DNA repair. Various clinical candidates have been identified with the role in PARP-1 inhibition. Based on the pharmacophoric features identified from previous studies and molecular docking interactions, thiazolidine-2,4-dione derivatives have been evaluated for their PARP inhibitory activity. From an in vitro assay, 5-((1-(4-isopropylbenzyl)-1H-indol-3-yl)methylene)thiazolidine-2,4-dione (16) was identified as a potent inhibitor having low micromolar inhibitory activity \((\hbox {IC}_{50} \,{=}\, 0.74 \,\pm \, 0.25\,\upmu \hbox {M})\). Thus, a structure-based design approach utilized in the present study helped to identify thiazolidine-2,4-dione as a novel scaffold against PARP-1 for potential development of potent anticancer therapeutics. 相似文献
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Eduardo Enciso Juan I. Sarmiento-Sánchez Héctor S. López-Moreno Adrián Ochoa-Terán Ulises Osuna-Martínez Evangelina Beltrán-López 《Molecular diversity》2016,20(4):821-828
The quinazolin-2,4-dione moiety is found in many compounds with important biological activities making it a target for its synthesis. In this work, a one-pot three-step synthesis of new quinazolin-2,4-diones from phthalic anhydrides and their activity against Leishmania mexicana are described. The new quinazolin-2,4-diones were isolated with yields in the range of 32–70 %. All compounds displayed lower cytotoxicity in RAW 264.7 macrophage over miltefosine. Compound 6,7-dichloro-3-phenylquinazoline-2,4(1H,3H)-dione (6e) displayed an attractive profile which includes anti-Leishmania mexicana activity (\(\hbox {IC}_{50} = 6.05\) \(\upmu \)M), much lower cytotoxic activity (\(\hbox {CC}_{50} = 111\) \(\upmu \)M) and a high selective index (\(\text {SI} = 18.35\)) proving to be superior to miltefosine. 相似文献
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合成了三种环氧孕甾衍生物:6-亚甲基-16α,17α-环氧孕甾-4-烯-3,20-二酮,6-甲基-16α,17α-环氧孕甾-4,6-二烯-3,20-二酮和6-甲基-16α,17α-环氧孕甾-4-烯-3,20-二酮。其中6-甲基-16α,17α-环氧孕甾-4,6-二烯-3,20-二酮未见文献报道。同时应用红光谱(FTIR)、紫外光谱(UV)、及核磁共振氢谱(1H NMR)对三种甾体化合物的结构进行了研究。结果表明,三种甾体化合物结构上的差异在FTIR,UV,1H NMR谱中有明显的特征并表现出一定的规律。 相似文献
19.
采用量子化学密度泛函理论(DFT)在B3LYP/6-311++G **水平上对环戊二烯与2(5H)-呋喃酮、丁烯二酸酐和2,5-二氢呋喃的Diels-Alder反应机理进行了理论研究,并且考虑了溶剂化效应和取代基效应对反应机理及能垒的影响。结果表明,本文所涉及的环戊二烯与二氢呋喃类化合物的Diels-Alder加成反应是以协同方式进行的;羰基取代基的吸电子作用是造成产物中C(1)-C(2)、C(3)-C(4)键键长增加的主要原因;反应所涉及到的FMO相互作用主要是环戊二烯的HOMO与二氢呋喃类化合物的LUMO之间的相互作用,羰基对反应活化能的影响主要是通过降低呋喃类化合物的LUMO能级,减小与环戊二烯的HOMO的能级差异,从而有利于反应进行的;反应2的活化能垒最低,从动力学的角度考虑在室温下可以进行。 相似文献