甲基对硫磷-D6的合成

报道了一种合成甲基对硫磷-D₆的新方法。以三氯硫磷、氘代甲醇和对硝基苯酚为起始原料,经三次酯化反应合成了目标产物甲基对硫磷-D₆,总收率47.6%,其结构经¹H NMR、 ¹³C NMR、 ³¹P NMR和HR-MS(ESI)确证。     

12,52-二羟基-15,55-二甲基-14,16,34,36,54,56,74,76-八硝基-2,4,6,8-四氧桥连-1,3,5,7（1,3）-杯[4]芳烃的合成

以1,5-二氟-2,4-二硝基苯和3,4,5-三甲氧基甲苯为起始原料,经环化、甲基化、硝化和去甲基化反应，合成了一种新型杯芳烃衍生物，其结构经¹H NMR，¹³C NMR，¹⁵N NMR和元素分析表征。      

铜催化α,β-不饱和羧酸与ICH2 CF3的脱羧偶联反应

铜催化下,以CH₃CN和HOAc为混合溶剂,α,β-不饱和羧酸与1,1,1-三氟-2-碘乙烷（ICH₂CF₃）发生脱羧偶联反应合成了一系列三氟乙基取代烯烃,其结构经¹H NMR、¹³C NMR和HR-MS确证。¹⁹F NMR分析显示该反应具有优良的立体选择性（E/Z最高为99/1）,分离收率最高达82%。     

Wittig/Michael串联反应高效合成含有磷叶立德的吲哚并喹唑啉酮衍生物

以吲哚并[2,1-b]喹唑啉-6,12-二酮（色胺酮）及三苯基膦乙酸乙酯（酯基磷叶立德）为原料,在二氯甲烷中反应2 h,经Wittig/Michael串联反应,以高达99%的收率一步合成了15个含有吲哚并喹唑啉骨架的磷叶立德衍生物。其代表产物的结构经X-ray单晶衍射进行确证,化合物结构经¹H NMR, ¹³C NMR, ³¹P NMR, ¹⁹F NMR和HR-MS（ESI-TOF）表征。     

Multilevel profiling and identification of Dalbergia odorifera and Dalbergia stevensonii by FTIR,NMR and GC/MS

Chemical differences of the extractives revealed by FTIR methods can be further confirmed by ¹H NMR and ¹³C NMR. Meanwhile, the volatile compounds in the extractives can be identified by GC/MS     

吲哚与含CF3氮杂对亚甲基苯醌的1,6-共轭加成反应合成含CF3的吲哚衍生物

以5 mol%布朗斯特酸(±)-BNPA为催化剂，含CF₃氮杂对亚甲基苯醌与吲哚为原料，通过1,6-共轭加成反应合成了7个结构新颖的含CF₃的吲哚类化合物，收率80%~87%，其结构经¹H NMR， ¹³C NMR， ¹⁹F NMR和HR-MS(ESI)表征，并对反应机理进行了探讨。     

新型含嘧啶的苯氧乙酸酯类衍生物的合成

以对羟基苯甲醛和一氯乙酸为起始原料,经羟醛缩合、关环及酯化等反应合成了6个含有嘧啶杂环的新型苯氧乙酸酯类衍生物,其结构经¹H NMR, ¹³C NMR, IR和HR-ESI-MS表征。     

新型菲并嗪类有机光伏材料的合成

以菲醌和邻位二胺为核心原料,经烷基化、硼化、Suzuki偶联、还原和关环反应合成了新型菲并嗪类有机光伏材料DTPZ,其结构经¹H NMR, ¹³C NMR, MALDI-TOF-MS和元素分析表征。     

Synthesis of new 4,6-diaryl-2-(arylthio)nicotinonitriles in Triton X-100 aqueous micellar media

In this communication,we report four component condensations of acetophenone,arylaldehydes,arylthiol,and malononitrile in the presence of Triton X-100（5 mol%） aqueous micelles.This reaction led to the formation of 4,6-diaryl-2-（arylthio）nicotinonitrile new derivatives in good yields.The FT-IR,¹⁹F NMR,¹H NMR,¹³C NMR spectra and elemental analysis confirm the structure of compounds.     

2-氯-4-苯基喹唑啉的合成

以邻苯甲酰苯甲酸为原料,依次经氯代、酰胺化、Hofmann重排、成环及氯化共5步反应合成了2-氯-4-苯基喹唑啉,总收率20.8%,其结构经¹H NMR和¹³C NMR确证。     

光谱法分析乙丙共聚物的序列结构及链节比

用FTIR, 1 H NMR和 13 C NMR分析乙丙共聚物的序列结构与链节比. 通过对乙丙共聚物 1 H NMR, 13 C NMR和 13 C-1 H二维核磁共振谱的综合分析, 提出了与前人不同的归属, 并提出了不同位置碳原子积分面积相关性分析方法, 该方法避免了烦琐的理论计算, 可简便地得到乙丙共聚物的主要序列结构. 通过比较 1 H NMR和 13 C NMR计算乙丙共聚物中乙烯、 丙烯链节比, 表明可以用 1 H NMR代替 13 C NMR完成对乙丙共聚物中乙烯、 丙烯链节比的定量计算.     

Flow injection analysis NMR (FIA–NMR): a novel flow NMR technique that complements LC–NMR and direct injection NMR (DI–NMR)

Details of a new flow NMR technique, flow injection analysis NMR (FIA–NMR), are presented for the first time. This method blends some aspects of both liquid chromatography–NMR and direct injection NMR, and complements both. FIA‐NMR is shown to be useful as an analytical technique, especially for repetitive analyses, and may also prove useful in the analysis of combinatorial chemistry libraries. The feasibility of FIA‐NMR is demonstrated by the quantitative analysis of an over‐the‐counter pharmaceutical. Copyright © 2003 John Wiley & Sons, Ltd.     

13C and 15N NMR studies of iron-bound cyanides of heme proteins and related model complexes: sensitive probe for detecting hydrogen-bonding interactions at the proximal and distal sides

Studies of the 13C and 15N NMR paramagnetic shifts of the iron-bound cyanides in the ferric cyanide forms of various heme proteins containing the proximal histidine and related model complexes are reported. The paramagnetic shifts of the 13C and 15N NMR signals of the iron-bound cyanide are not significantly affected by the substitution of the porphyrin side chains. On the other hand, the paramagnetic shifts of both the 13C and 15N NMR signals decrease with an increase in the donor effect of the proximal ligand, and the 13C NMR signal is more sensitive to a modification of the donor effect of the proximal ligand than the 15N NMR signal. With the tilt of the iron-imidazole bond, the paramagnetic shift of the 13C NMR signal increases, whereas that of the 15N NMR signal decreases. The hydrogen-bonding interaction of the iron-bound cyanide with a solvent decreases the paramagnetic shift of both 13C and 15N NMR signals, and the effect is more pronounced for the 15N NMR signal. Data on the 13C and 15N NMR signals of iron-bound cyanide for various heme proteins are also reported and analyzed in detail. Substantial differences in the 13C and 15N NMR shifts for the heme proteins can be explained on the basis of the results for the model complexes and structures around the heme in the heme proteins. The findings herein show that the paramagnetic shift of the 13C NMR signal of the iron-bound cyanide is a good probe to estimate the donor effect of the proximal imidazole and that the ratio of 15N/13C NMR shifts allows the hydrogen-bonding interaction on the distal side to be estimated.     

NMR Imaging and materials research

The use of nuclear magnetic resonance in materials research is elaborated. While NMR applications to materials are discriminated between rigidly solid, rubbery, and liquid matter, NMR methods are divided into spectroscopy and imaging. The connections between the different material and NMR categories are explained. Particular emphasis is placed on NMR with spatial resolution, which is illustrated by examples from imaging of solid polymers and elastomers.     

Hyphenation of capillary separations with nuclear magnetic resonance spectroscopy

The hyphenation of small-volume separations to information-rich detection offers the promise of unmatched analytical information on the components of complex mixtures. Nuclear magnetic resonance (NMR) spectroscopy provides information about molecular structure, although sensitivity remains an issue for on-line NMR detection. This is especially true when hyphenating NMR to capillary separations as the observation time and analyte mass are decreased to the point where reduced information is obtained from the eluting analytes. Because of these limitations, advances in instrumental performance have a large impact on the overall performance of a separation–NMR system. Instrumental aspects and the capabilities of cLC–NMR, CEC–NMR and CE–NMR are reviewed, and applications that have used this technology highlighted. Recent trends towards small volume capillary scale separations are emphasized, as is the recent success of capillary-isotachophoresis (cITP)–NMR.     

NMR位移试剂Eu(fod)~4^-对锍盐^1H和^1^3C NMR的影响

合成了八种新的四氟硼酸二甲基苯基锍，用元素分析和核磁共振对其结构进行了表征。研究了以CDCl~3为溶剂，NMR位移试剂Eu(fod)~4^-对所合成锍盐的^1H和^1^3C NMR的影响。结果表明，Eu(fod)~4^-是一个对锍盐非常有效的位移试剂，且Eu(fod)~4^-对二甲基苯基锍盐之甲基的^1H和^1^3C NMR的位移呈线性关系。     

HR-MAS NMR Applications in Plant Metabolomics

Metabolomics is used to reduce the complexity of plants and to understand the underlying pathways of the plant phenotype. The metabolic profile of plants can be obtained by mass spectrometry or liquid-state NMR. The extraction of metabolites from the sample is necessary for both techniques to obtain the metabolic profile. This extraction step can be eliminated by making use of high-resolution magic angle spinning (HR-MAS) NMR. In this review, an HR-MAS NMR-based workflow is described in more detail, including used pulse sequences in metabolomics. The pre-processing steps of one-dimensional HR-MAS NMR spectra are presented, including spectral alignment, baseline correction, bucketing, normalisation and scaling procedures. We also highlight some of the models which can be used to perform multivariate analysis on the HR-MAS NMR spectra. Finally, applications of HR-MAS NMR in plant metabolomics are described and show that HR-MAS NMR is a powerful tool for plant metabolomics studies.     

Fragment Screening and Fast Micromolar Detection on a Benchtop NMR Spectrometer Boosted by Photoinduced Hyperpolarization

Fragment-based drug design is a well-established strategy for rational drug design, with nuclear magnetic resonance (NMR) on high-field spectrometers as the method of reference for screening and hit validation. However, high-field NMR spectrometers are not only expensive, but require specialized maintenance, dedicated space, and depend on liquid helium cooling which became critical over the recurring global helium shortages. We propose an alternative to high-field NMR screening by applying the recently developed approach of fragment screening by photoinduced hyperpolarized NMR on a cryogen-free 80 MHz benchtop NMR spectrometer yielding signal enhancements of up to three orders in magnitude. It is demonstrated that it is possible to discover new hits and kick-off drug design using a benchtop NMR spectrometer at low micromolar concentrations of both protein and ligand. The approach presented performs at higher speed than state-of-the-art high-field NMR approaches while exhibiting a limit of detection in the nanomolar range. Photoinduced hyperpolarization is known to be inexpensive and simple to be implemented, which aligns greatly with the philosophy of benchtop NMR spectrometers. These findings open the way for the use of benchtop NMR in near-physiological conditions for drug design and further life science applications.     

NMR Studies of polymeric materials - an overview

NMR has been used extensively in studies of synthetic polymers. The approaches employed may require solution NMR, solid state NMR, or NMR imaging. In each case, different techniques and analytical methodologies have been devised to facilitate experimentation or to maximize information output. These techniques are not mutually exclusive and often provide complementary information. A selective review is made herewith of polymer/NMR studies, with emphasis on the contributions made at NMR symposia held in Detroit in October, 1993 as part of the 20th FACSS meeting.     

Dry‐cured ham tissue characterization by fast field cycling NMR relaxometry and quantitative magnetization transfer

Fast field cycling (FFC) and quantitative magnetization transfer (qMT) NMR methods are two powerful tools in NMR analysis of biological tissues. The qMT method is well established in biomedical NMR applications, while the FFC method is often used in investigations of molecular dynamics on which longitudinal NMR relaxation times of the investigated material critically depend. Despite their proven analytical potential, these two methods were rarely used in NMR studies of food, especially when combined together. In our study, we demonstrate the feasibility of a combined FFC/qMT‐NMR approach for the fast and nondestructive characterization of dry‐curing ham tissues differing by protein content. The characterization is based on quantifying the pure quadrupolar peak area (area under the quadrupolar contribution of dispersion curve obtained by FFC‐NMR) and the restricted magnetization pool size (obtained by qMT‐NMR). Both quantities correlate well with concentration of partially immobilized, nitrogen‐containing and proton magnetization exchanging muscle proteins. Therefore, these two quantities could serve as potential markers for dry‐curing process monitoring. Copyright © 2016 John Wiley & Sons, Ltd.