The 1H And 2H NMR Spectra Of HFeCo3 (CO)12

The detection of the ²H resonance of ²HfeCo₃ (CO)₁₂ led to the detection of the broader ₁H resonance of the ₁H isotopomer. The shift is -21.4 ppm.     

Hg(PMBP)2(HPMBP)2和Zn(PMBP)(H2O)Cl配合物的合成及结构

用1-苯基-3-甲基-4-苯甲酰基吡唑啉酮-5(HPMBP)与HgCl₂和ZnCl₂·6H₂O作用,分别合成化学式为[Hg(PMBP)₂(HPMBP)₂]和[Zn(PMBP)(H₂O)Cl]的配合物;用元素分析、IR、¹HNMR和电导等物理化学方法推测了配合物的分子结构式。配体在此螯合过程中皆由酮式转变为烯醇式,在Hg(Ⅱ)配合物中部分不变。     

Deuterated Epoxides and Their Polymers. I. Synthesis of cis- and trans-Propylene Oxide-1-d and Their NMR Spectra

Abstract

cis- and trans-Propylene oxide-1-d were synthesized from the corresponding propenyl halides via propenyllithium and propylene bromohydrin. Their NMR spectra (about 3% in benzene) were analyzed in terms of ABX₃ spin system and the assignment was carried out. The chemical shift of the methylene proton in cis position to the methyl group was found to be Δ = 1.86 ppm and that of the methylene proton in trans position Δ = 2.18 ppm (downfield from HMDS). The H-D couplings were observed in the methine-methylene part spectra decoupled from methyl protons. The observed J_HD's agree with the theoretical relation: J_HH = 6.5 14 X J_HD.     

碘杂环化合物的1H NMR谱研究

碘杂环类化合物的合成及性质已有报导[1-4],但碘杂环中碘作为正离子的¹HNMR谱报导较少。由于碘正离子诱导效应的结果,使环上相邻质子的化学位移向低场移动,这主要是碘正离子吸引电子的结果,使相邻质子的电子云密度降低,化学位移向低场移动。本文报导了19个碘取代及碘杂环化合物的¹HNMR谱,这种类型化合物的¹HNMR谱未见过系统报导。     

1-苯基-3-(3'-吲哚基)-5-取代苯基-2-吡唑啉的合成及1H NMR和MS中的取代基效应

J-(3'-吲哚基)-3-取代苯基-2-丙烯-1-酮与茉肼反应,合成了10种新的1-苯基-3-(3'-吲哚基)-5-取代苯基-2-吡唑啉衍生物,其结构通过各种波谱证实.讨论了此系列化合物¹HNMR和Ms中的取代基效应,得出取代基常数σ或σ⁺与质子化学位移,碎片相对丰度之间存在着良好的线性关系.     

两个特殊骨架的C_(20)－二萜生物碱的全部~1H(~(13)C)核磁共振信号指定

两个具有特殊骨架的C_(20)-二萜生物碱北乌灵（kusnezoline）和峨翠灵（ omeieline）分别分自中国特产毛茛科植物北草乌（Aconitum hkusnezoffii Paritz）、彭州岩乌头（A. racemulosum var. pengzhouense）和峨眉翠雀花（ Delphinium omeiense W. T. Wang）。应用2D NMR技术(~1H-~1H COSY, HMQC, HMBC, NOESY)全面归属了这两个生物碱的~1H和~(13)C信号的化学位移。     

BINOL Aza Macrocycle Derivatives: Synthesis of Dinaphthosulfone Aza Macrocycles Using p-Toluenesulfonic Acid (p-TsOH) in Methanol as an Efficient Route and Evaluation of Their 1H NMR Spectra

Dinaphthosulfone aza macrocycles were synthesized from the reaction of diamines and dinaphthosulfone diester (1,1′-sulfoxobis-(2-naphthoxy(2-methyl acetate))) in methanol in the presence of catalytic amounts of para toluenesulfonic acid (p-TsOH). Dinaphthosulfone diester (1,1′-sulfoxobis-(2-naphthoxy(2-methyl acetate))) was synthesized from the corresponding dinaphthosulfide diester and hydrogen peroxide in formic acid at room temperature. Dinaphthosulfide diester was prepared from initial dinaphtholsulfide diol (1,1′-thio bis(2-hydroxy naphthalene)) and methylchloroacetate. ¹H NMR spectroscopy showed the unusual splittings for these dinaphthosulfone aza macrocycles, and this finding could be proposed as the role of tetrahedral structure of sulfone functional group, hydrogen bonding in the cavity and size of macrocycle.     

3-亚甲基异苯并呋喃-1(3H)-酮及其衍生物的合成研究

以2-乙烯基苯甲酸甲酯及其衍生物为原料,经过酯水解反应,随后发生环氧化、环合反应制备了3-羟甲基异苯并呋喃-1(3H)-酮及其衍生物;再和三溴化磷或者对甲苯磺酰氯发生亲核取代,最后通过消除反应合成了3-亚甲基异苯并呋喃-1(3H)-酮及其衍生物.在亲核取代和消除反应中,对甲苯磺酰氯法比三溴化磷法产率高.目标产物及其中间体有10个是新化合物.化合物结构用1H NMR,13C NMR,MS和IR表征.目标产物在空气中长期放置没有发生二聚.     

meso和dl 2,3-二氰基-2,3-二(p-取代苯基)丁二酸二乙酯的~1H NMR研究

测定了meso和dl 2,3-二氰基-2,3-二(p-X苯基)丁二酸二乙酯(X=OCH_3,CH_3,H,Cl,NO_2)的~1H NMR谱及X为CH_3相应二乙酯的~1H Noesy谱。在meso和dl异构体中,苯环m-~1H的化学位移与p-X的Hammett基团常数σ呈线性关系,c~1H的化学位移仅受分子构型的影响,;△δdl-meso为负值,乙氧基中CH_2和CH_3的质子化学位移也只受分子构型的影响,△δdl-meso均为正值。     

Concentration effects on the1H NMR parameters of rhodamine 6G

Kaliningrad State University. Translated fromZhurnal Struktumoi Khimii, Vol. 36, No. 4, pp. 756–760, July–August, 1995.     

两种中位不对称四苯基卟啉的氢谱解析

剖析两种结构不对称氰基取代四苯基卟啉(5-对氰基苯基-10,15,20-三对甲基苯基卟啉(triCH3,CN-TPP)和5-对甲基苯基-10,15,20-三对氰基苯基卟啉(triCN,CH3-TPP)的核磁共振氢谱。     

Synthesis and properties of 1,4,8,11,15,18,22,25-octaalkoxy-2,3,9,10,16,17,23,24-octakis(phenylthio)phthalocyaninato copper(II)

1,4,8,11,15,18,22,25-Octaalkoxy-2,3,9,10,16,17,23,24-octakis(phenylthio)phthalocyaninato copper(II) was synthesized. They were easily soluble in organic solvents and their Q-bands showed bathochromic shifts about 100 nm compared with unsubstituted phthalocyaninato copper(II). Their properties were examined.     

NMR Determination of the Microstructure of Polyvinyl Chloride Sulfone). II. 13C-(1H) Spectra

The ¹³C-(¹H) NMR spectra of poly(vinyl chloride sulfone)s with macroscopic compositions corresponding to the ratio vinyl chloride (V):SO₂(S) = n from ca. 1 to 4 have been analyzed in terms of comonomer sequences and configurational placements. In the copolymer with n ? 1, methylene and methine carbons in SVS sequences were resolved and were sensitive to “across SO₂” tacticity. No SVS sequences were observed in the copolymer with n = 2.0, confirming that it had a regular SVVS structure, which also showed a high “internal” stereosequence regularity. It was not possible to discriminate the methylene or methine carbon atoms in S(V)_n S sequences with n ≥ 2.     

Substituent effect on the 1H NMR Spectra of trans aryl methyl oxiranes and arylpropenes

The ¹H NMR spectra of 1-aryl-2-methyl oxiranes substituted in the phenyl ring and of the corresponding vinyl derivatives have been analysed. The substituent effect on oxiran protons seems mostly polar in character, as shown by correlations with substituent constants, solvent effects and the fact that perturbation decreases with increasing distance from the substituent. The comparison with the corresponding vinyl derivatives, in which conjugation effects are present, confirms this point. The results also seem to exclude the possibility of substituents causing significant changes on the preferred conformation of the phenyl ring. Ring current contributions on oxirane protons, evaluated by SCF procedure, show that their change with substituents is very small and does not represent a significant part of the change of proton chemical shift with substituents.     

Boosting the Resolution of 1H NMR Spectra by Homonuclear Broadband Decoupling

Broadband homonuclear decoupling of proton spectra, that is, the collapse of all multiplets into singlets, has the potential of boosting the resolution of ¹H NMR spectra. Several methods have been described in the last 40 years to achieve this goal. Most of them can only be applied in the indirect dimension of multi‐dimensional NMR spectra or special data processing is necessary to yield decoupled 1D proton spectra. Recently, complete decoupling of proton spectra during acquisition has been introduced; this not only significantly reduced the experimental time to record these spectra, but also removed the need for any sophisticated processing schemes. Here we present an introduction and overview of the techniques and applications of broadband proton‐decoupled proton experiments.     

An Efficient One-Pot Synthesis of 2,3-Dialkyl-1,1-Diethyl-1-(Acetylamino)-3-(1,1,1-Triphenylphosphanilidene)-1,1,2,3-Propanetetracarboxylates and Their Temperature-Dependent NMR Spectra

Abstract

Stable crystalline phosphorus ylides of 1,1-diethyl 2,3-dimethyl 1-(acetylamino)-3-(1,1,1-triphenylphosphanilidine)-1,1,2,3-propanetetracarboxylates were obtained in excellent yields from the 1:1:1 addition reaction between triphenylphosphine and dialkyl acetylenedicarboxylates in the presence of diethyl acetamidomalonate as a CH-acid. These stable ylides exist in solution as a mixture of two geometrical isomers (E and Z) as a result of restricted rotation around the carbon–carbon partial double bond resulting from conjugation of the ylide moiety with the adjacent carbonyl group on the nuclear magnetic resonance (NMR) time scale at ambient temperature. The dynamic effects in the ylide moieties were investigated by ¹H NMR spectra.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

An Efficient One-Pot Synthesis and Temperature Dependence of NMR Spectra of Nitrogen-Containing Phosphorus Ylides

The addition of triphenylphosphine to dialkyl acetylenedicarboxylates in the presence of trifluoroacetamide, a NH acid, leads to stable crystalline phosphorus ylides in exellent yields. These stable ylides exist as a mixture of two geometrical isomers as a result of restricted rotation around the carbon-carbon partial double bond, resulting from conjugation of the ylide moiety with the adjacent group.     

Synthesis and NMR (1H and 13C) Studies of azole analogs of diclofurime

The synthesis, structure elucidation and chemotherapeutic activity of novel heterocyclic analogues of the cardiotropic agent Diclofurime are reported.     

焦脱镁叶绿酸-a甲酯衍生物的合成及其结构与光谱性能关系研究

以焦脱镁叶绿酸-a甲酯(MPP-a, 1)为起始原料,通过乙二醇对E-环羰基进行保护,选用四氧化锇和高碘酸钠将3-位碳碳双键氧化,生成131-二氧环戊基-131-去氧焦脱镁叶绿酸-d甲酯(2),经Grignard反应将3-甲酰基转换成羟烷基得仲醇3,再通过高钌酸四乙基胺和N-甲基吗啡啉N-氧化物将其氧化成酮4,脱去保护基生成3-烷酰基3-去乙烯基焦脱镁叶绿酸-a甲酯(6).焦脱镁叶绿酸-d (MPP-d)7与过量重氮甲烷发生加成和重排反应,生成6a及3-烷酰甲基3-去乙烯焦脱镁叶绿酸甲酯衍生物8和9,7的3-位醛基经过Wittig和氧化反应得到3-苯乙二酰基焦脱镁叶绿酸甲酯11.所合成的新卟吩衍生物均经UV,IR,¹H NMR及元素分析证明其结构,并且讨论了周边取代羰基对核磁共振光谱和最大可见光吸收的影响.