共查询到19条相似文献,搜索用时 109 毫秒
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本文对强效镇痛剂羟甲芬太尼(OMF)八个对映异构体中的其中四个, 即(-)-cis-(3R,4S,2'R)-OMF (1), (+)-cis-(3-R,4S,2'S)-OMF (2),(+)-trans-(3S,4S,2'R)-OMF (3), 和(+)-trans-(3S,4S,2'S)-OMF (4)进行了^1HNMR研究, 归属了所有的共振谱线。对哌啶环质子间偶合常数的分析表明, 所有顺式和反式异构体中的哌啶环都呈现相同的椅式构象。在顺式异构体中3-甲基位于直立键, 而4-N-苯基丙酰胺基位于平伏键, 反式异构体中它们均位于平伏键。讨论了3-甲基和4-N-苯基丙酰胺基的立体取代对NMR的影响, 在顺式异构体中4-N-苯基丙酰胺基的构象相对固定, 而在反式异构体中则较为自由。 相似文献
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^1H NMR选择检测新技术用于新三萜皂苷的结构研究 总被引:3,自引:0,他引:3
从中药川续断根部的乙醇提取物中分得1个新的三萜皂苷,经过测定,其结构为:3-O-α-L-吡喃鼠李糖(1--3)-β-D-吡喃葡萄糖(1--3)-β-L-吡喃鼠李糖(1--2)-β-L-吡喃阿拉伯糖-常春藤苷元(1).研究表明,采用一维SEMDY和三照射NOE差谱NMR新技术相结合能以"拼凑"方式,测定糖链结构.方法简便、快速、测定结果可靠,重叠的信号可以指认,并且对样品不必进行化学降解或衍生化.本方法也可以用于其他类型的寡糖结构测定。 相似文献
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测定了各pD值下BPHA[BPHA是N,N'-bis(2-aminoethyl)-1,3-propanediaminehexaaceticacid的简称,中文名称为二胺乙基丙二胺六乙酸]和Zn^2^+-BPHA的^1HNMR谱。BPHA两端羧甲基上亚甲基质子的化学位移δ~a和中间羧甲基上亚甲基质子的化学位移δ~b随pD值交替变化。Zn^2^+-BPHA的^1HNMR谱有3种情况:pD<6,对应Zn(II)-H~2BPHA^4^-,有一特征尖峰,显示自由-NH^+(CH~2COO^-)~2残基存在;pD=6-9,对应Zn(II)-HBPHA^5^-,该峰消失,显示4个胺基全部配位;pD>9,对应Zn(II)-BPHA^6^-,该峰再次出现,1个N(CH~2COO^-)~2脱离配位体系。在3种形态的配合物中,Zn-N键都是非活性的,Zn-O键在后两种形态配合物中是非活性的。 相似文献
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香茶菜属二萜类化合物的1H NMR 研究 总被引:1,自引:0,他引:1
通过对二十三个香茶菜植物中二萜类化合物的1HNMR 参数的归纳, 总结了这些化合物的主要质子信号的规律, 用分子模型使分子立体结构(B,C 环构象和取代基构型)与峰形相关连, 为此类化合物的签别和结构确定提供了依据. 相似文献
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重水中固氮酶催化还原乙炔产物的^1H NMR研究 总被引:2,自引:0,他引:2
用^1HNMR研究了固氮酶在重水中催化还原乙炔的反应产物氘代乙烯.种用群对称性对^1HNMR谱图进行了归属,计算了几种可能的C`2H~2D~2结构以及C~2H~3D结构的NMR谱线频和强度,得出了理论谱.通过理论谱与实验谱的比较,表明固氮酶在重水中催化还原乙炔的产物主要以顺式结构C~2H~2D~2为主,并含有较多的单氘代烯.单氘代乙烯相对乙烯的化学位移往高场移动约4.0Hz,而双氘代乙烯向高场的位移大约是单氘代乙烯的2倍左右。 相似文献
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测定了各pD值下BPHA[BPHA是N,N'-bis(2-aminoethyl)-1,3-propanediaminehexaaceticacid的简称,中文名称为二胺乙基丙二胺六乙酸]和Zn^2^+-BPHA的^1HNMR谱。BPHA两端羧甲基上亚甲基质子的化学位移δ~a和中间羧甲基上亚甲基质子的化学位移δ~b随pD值交替变化。Zn^2^+-BPHA的^1HNMR谱有3种情况:pD<6,对应Zn(II)-H~2BPHA^4^-,有一特征尖峰,显示自由-NH^+(CH~2COO^-)~2残基存在;pD=6-9,对应Zn(II)-HBPHA^5^-,该峰消失,显示4个胺基全部配位;pD>9,对应Zn(II)-BPHA^6^-,该峰再次出现,1个N(CH~2COO^-)~2脱离配位体系。在3种形态的配合物中,Zn-N键都是非活性的,Zn-O键在后两种形态配合物中是非活性的。 相似文献
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本工作用配位平衡和快交换方法定量描述了二氧六环水体系中^1H和^1^7O化学位移随浓度的变化. 讨论了未配位水的结构破坏程度及其存在形式. 相似文献
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Determination of pKa values of some novel benzimidazole salts by using a new approach with 1H NMR spectroscopy
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Benzimidazoles and their derivatives including imidazole are studied widely because they exist in the structure of natural products and different drugs. pKa values are extremely important for drug discovery and improvement in order to determine pharmacokinetic and pharmacodynamic features such as permeation through biological barriers, interactions with the target area or side effects. Acid–base features (pKa) have great importance not only for physiological characteristics but also for being used as a ligand or changing physico‐chemical features by turning benzimidazoles into salts. Within the scope of this study, a variety of new benzimidazole salts were synthesized, and their characterizations were made by NMR spectroscopy, FTIR spectroscopy and element analysis techniques. The pKa values of synthesized benzimidazole salts were determined by inflection point approach using integration values obtained with 1H NMR spectroscopy and Henderson–Hasselbalch analysis. pKa values of some benzimidazole salts were also determined by potentiometric methods in order to compare those of NMR spectroscopy results. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
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《Magnetic resonance in chemistry : MRC》2003,41(9):729-730
The characterization of four aryl diisoprenes was carried out by 1D‐ and 2D‐NMR methods, which permitted the assignment of the signals of all protons and all carbon atoms. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
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Yoshio Nakahara Tsutomu Takeuchi Shoutaro Yokoyama Keiichi Kimura 《Surface and interface analysis : SIA》2011,43(4):809-815
Quantitative analysis of reacted silanol groups in silica nanoparticles modified chemically with monochlorosilanes was performed by 1H NMR after treatment with cesium fluoride. Silica nanoparticles were modified chemically by the reaction between the silanol groups and monochlorosilanes, and the structure of the organic moiety anchored onto the silica surface was confirmed with solid‐state 13C NMR. As monochlorosilanes react with silanol groups at 1:1 ratio unlike di‐ or trichlorosilanes, the number of the silanes introduced into silica nanoparticles equals that of reacted silanol groups. Organically modified silica nanoparticles were dissolved using cesium fluoride, and the amount of the soluble organic compounds originated from the introduced silanes was determined by a 1H NMR internal standard method using pyrene as the reference. Those values determined by 1H NMR were in good agreement with those determined by elemental analysis. Thus, the number of reacted silanol groups per one particle was calculated on the basis of the results obtained by the 1H NMR method, and the values were highly dependent on the steric structure of the introduced silanes. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
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A detailed analysis of the proton high-field NMR spectra of vinegars (in particular of Italian balsamic vinegars) is reported. A large number of organic substances belonging to different classes, such as carbohydrates, alcohols, organic acids, volatile compounds and amino acids, were assigned. The possibility of quantification of the substances identified in the whole vinegar sample, without extraction or pre-concentration steps, was also tested. The data validity was demonstrated in terms of precision, accuracy, repeatability and inter-day reproducibility. The effects of the most critical experimental parameters (sample concentration, water suppression and relaxation time) on the analysis response were also discussed. 1H NMR results were compared with those obtained by traditional techniques (GC-MS, titrations), and good correlations were obtained. The results showed that 1H NMR with water suppression allows a rapid, simultaneous determination of carbohydrates (glucose and fructose), organic acids (acetic, formic, lactic, malic, citric, succinic and tartaric acids), alcohols and polyols (ethanol, acetoin, 2,3-butanediol, hydroxymethylfurfural), and volatile substances (ethyl acetate) in vinegar samples. On the contrary, the amino acid determination without sample pre-concentration was critical. The 1H NMR method proposed was applied to different samples of vinegars, allowing, in particular, the discrimination of vinegars and balsamic vinegars. 相似文献
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The 1H and 13C NMR spectra of methylenecyclopropane, both in the isotropic phase and in the Merck IV nematic phase, were analysed. The relative signs of the 13C H scalar coupling constants were determined. The complete geometry deduced from this study was compared with that from a microwave study, and the discrepancies are discussed. 相似文献
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Nine flavonol derivatives were studied. Previously reported NMR data of three of these derivatives were corrected. We report complete assignments of the NMR data for six flavonol derivatives not previously studied. 相似文献
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Test‐separator units, as traditional methods of well surveillance, mainly suffer from their inherent constraints including the expensive instrumental, mechanical, electrical, piping and safety devices along with technical and protective inspections, repair and operation services, facilities and infrastructures. Other problems are time and cost consuming, uncertainty of well isolation in test separator and need to close the co‐line wells, which are diminished using multivariate thermal well testing. A novel approach was proposed and tested to classify the oil samples taken from individual wells by source and type. The novelties of this work were the use of the applied aspects of 1H NMR spectroscopy in petroleum upstream engineering, the replacement of traditional test methods, the improvement of the confidence of tests and the recognition of multisource streams. The weighed sum method was used to correlate the spectra information, taken from the samples of Iranian offshore oil wells. The experimental results and the field data revealed that the present approach was appropriate for precocious, quick and reliable surveillance of individual oil wells located in an oil field. The model was supported by field experiments and has predicted the accurate productivity of oil wells with respect to the current expensive techniques since 2010. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献