含R_2NCS_2配体的过渡金属配合物~1H NMR研究

报道１１中含Ｒ_２ＮＣＳ_２配体的过渡金属配合物的~１ＨＮＭＲ研究结果。对其顺磁性化合物的磁性和电子结构进行了讨论；并探讨了抗磁性化合物的分子结构和ＮＭＲ关系。     

六氟磷酸二(2,2'-联吡啶)·(4,4'-二甲基-2,2'-联吡啶) 合钌(Ⅱ)的二维核磁共振谱分析

用一维NMR方法研究了电化学发光物质六氟磷酸二(2,2'-联吡啶)·(4,4'-二甲基-2,2'-联吡啶)合钌(Ⅱ)的立体结构,借助二维1H-1H COSY和1H-13C COSY实验技术对其氢谱和碳谱进行了完全的归属,并给出了其氢谱和碳谱的化学位移值.     

Molecular dynamics in paramagnetic materials as studied by magic-angle spinning 2H NMR spectra

A magic-angle spinning (MAS) 2H NMR experiment was applied to study the molecular motion in paramagnetic compounds. The temperature dependences of 2H MAS NMR spectra were measured for paramagnetic [M(H2O)6][SiF6] (M=Ni2+, Mn2+, Co2+) and diamagnetic [Zn(H2O)6][SiF6]. The paramagnetic compounds exhibited an asymmetric line shape in 2H MAS NMR spectra because of the electron-nuclear dipolar coupling. The drastic changes in the shape of spinning sideband patterns and in the line width of spinning sidebands due to the 180 degrees flip of water molecules and the reorientation of [M(H2O)6]2+ about its C3 axis were observed. In the paramagnetic compounds, paramagnetic spin-spin relaxation and anisotropic g-factor result in additional linebroadening of each of the spinning sidebands. The spectral simulation of MAS 2H NMR, including the effects of paramagnetic shift and anisotropic spin-spin relaxation due to electron-nuclear dipolar coupling and anisotropic g-factor, was performed for several molecular motions. Information about molecular motions in the dynamic range of 10(2) s(-1)相似文献   

Synthesis of 3—Biaryl—1—ferrocenyl—2—propene—1—ones

The novel structures of organometallic compounds 3-biaryl-1-ferrocenyl-2-propene-1-ones 5 were synthesized for nonlinear optical chromophores by Suzuki cross-coupling reaction.Their structures were determined with elemental analyses,^1H NMR spectra and ^13C NMR spectra.     

一些单立方烷化合物MFe_3S_4(S_2CNR_2)_5(M=Mo,W)的~1H NMR研究

本文报道了一些单立方烷化合物MFe_3S_4(S_2CNR_2)_5(M=Mo,W;R_2=Me_2,Et_2,C_4H_8,OC_4H_8,C_5H_(10))的~1H NMR谱研究,结果表明与铁原子相连的配体的α-H产生了相当大的各向同性位移,它随温度升高而减少,基本上服从居里定律。本文还讨论了化合物中的配体间交换反应以及簇骼中金属原子间耦合作用对配体的NMR的影响。     

含手性膦配体2-MBPA铂(Ⅱ)配合物的2DNMR

利用一维和二维ＮＭＲ技术,对含有手性膦配体的铂配合物ｃｉｓ－〔Ｐｔ（２－ＭＢＰＡＨ）２Ｃｌ２〕（１）,ｔｒａｎｓ－〔Ｐｔ（２－ＭＢＰＡＨ）２Ｃｌ２〕（２）,ｃｉｓ－〔Ｐｔ（２－ＭＢＰＡ）２〕（３）和ｃｉｓ－〔Ｐｔ（２－ＭＢＰＡ）（２－ＭＢＰＡＨ）Ｃｌ〕（４）进行１Ｈ和１３ＣＮＭＲ谱分析,区分了化合物（３）和（４）,归属了糖苷部分的１Ｈ和１３ＣＮＭＲ谱线,并根据磷和铂及磷与磷的偶合常数确定化合物（３）和（４）是顺式构型     

Structural assignment of regioisomeric 3-[2- or 5-anilino-2-(alkylamino)phenyl]propanoic acids, 2H-1,4-benzothiazin-3(4H)-ones and 2,3-dihydro-1,5-benzothiazepin-4(5H)-ones by 1D NOE and gHMBC NMR techniques

The 1H and 13C NMR spectra of compounds 1-11 and 16-22 in CDCl3 and DMSO-d6 solutions allowed structural assignment to regioisomers 1/5 and 2/6 and their regioselective cyclization products 16-18 utilizing one- and two-dimensional NMR techniques (APT, DEPT, NOE difference, COSY, NOESY, HETCOR and gHMQC, gHMBC). Temperature-dependent 1H NMR spectra of 8-anilino-5-(4-methyl-2-pentyl)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one (18) indicated a free energy of activation (deltaG++) of ca 17 kcal mol(-1) for interconversion between rotamers. The 1H and 13C NMR spectra of 20 and 22 containing two chiral centers exhibit duplication of several signals, indicating the existence of two diastereomeric forms. The structure of 4 was unambiguously confirmed by x-ray crystallography.     

核磁共振方法表征2,2''''-二(对羧酸苯氧基)-1,1''''联萘

利用１Ｈ ＮＭＲ，１３Ｃ ＮＭＲ研究了 ２，２’－二（对羧酸苯氧基）－１，１’－联萘结构，并通过１Ｈ－１Ｈ ＣＯＳＹ及１３Ｃ－１Ｈ异核相关谱进一步确定了其１Ｈ谱和１３Ｃ谱中各谱峰的归属，为同类化合物的表征提供了一个依据。     

含二氮杂萘酮单元双官能团化合物结构的波谱表征

在成功地合成了11个用于制备聚芳酰胺类聚合物的含二氮杂萘酮单元的双官能团化合物基础上,本实验用核磁共振波谱确定了各化合物的结构。用二维同核位移相关谱(gCOSY)、异核^13C-^1H-键相关谱(gHSQC)和异核^13C-^1H远程相关谱(gHMBC)完成了全部^1H和^13C NMR谱带的归属;首次报道了该系列衍生物的氢和碳原子的化学位移值。对其系列化合物的核磁共振波谱及红外光谱的特征进行了讨论。     

2-卤-3-氨基-2-烯丙亚胺化合物的合成

由具有2位氢的3-氨基-2-烯丙亚胺与N-氯或N-溴琥珀酰亚胺以甲苯作溶剂在常温下反应，制备了-些未见文献报道的2-氯和2-溴-3-氨基-2-烯丙亚胺，化合物结构均经元素分析，^1H NMR，^13C NMR和MS确证。     

微波诱导下2-芳氧甲基苯并咪唑-1-水杨醛乙酰腙衍生物合成及生物活性研究

在微波辐射条件下, 通过2-芳氧甲基苯并咪唑-1-乙酰肼衍生物与水杨醛进行缩合反应, 合成了10种未见文献报道的2-芳氧甲基苯并咪唑-1-水杨醛乙酰腙衍生物. 它们的结构经元素分析, IR, ¹H NMR和¹³C NMR确证. 初步生物活性试验结果表明该系列化合物对小麦幼苗的生长具有明显的调节作用.     

[2+2]型Schiff碱大环化合物及其配合物的合成

利用Mn2 ,Ba2 作为模板离子,合成了一类新型的Schiff碱型大环化合物,Mn2 用于L1和L2的合成,并在洗涤时自动解络,L3和L4的合成以Ba2 为模板.L3和L4的Ba2 配合物经与Na2SO水溶液反应解络,得到自由配体L3和L4.上述大环配体和各种配合物均经元素分析,IR,1H NMR,MS等证实了它们的结构和组成.     

Carbon-13 nuclear magnetic resonance spectra of methyl 2-pyronecarboxylates

The ¹³C NMR spectra of methyl 2-pyrone-3-, 4-, 5- and 6-carboxylates were studied and the substituent effects on the 2-pyrone ring were compared with those of some model compounds. ¹H NMR spectra were also recorded and discussed. The long range ¹³C, ¹H coupling constants were obtained, discussed and proved useful in signal assignments.     

A 13C and 1H NMR study of diastereomeric α-methylidene-β-hydroxy-γ-alkoxy esters

The ¹³C and ¹H NMR spectra of α-methylidene-β-hydroxy-γ-alkoxy-pentanoates and -decanoates are presented. These data are consistent with a preferred conformation in which an intramolecular hydrogen bond is present. Very characteristic steric shifts in the ¹³C and ¹H NMR spectra provide an efficient tool for the configurational assignment for this class of compounds.     

内式及外式-5,5-二取代-3-氧代-4-氧杂三环[5,2,1,02,6]-8-癸烯类化合物的合成

由于许多降冰片烷衍生物及内酯类化合物都是很好的香原料,可用于调制化妆品或食用香精。为了探讨结构与香气的关系,并寻找新型的香原料,我们将上述两部分骨架-降冰片烷环系及内酯环系结合在一起,合成了具有如下结构的化合物16个。     

The 1H NMR spectra of p-substituted phenyl 2-chloro-2-fluoroethyl sulphides

The 60 MHz ¹H NMR spectra of p-substituted phenyl 2-chloro-2-fluoroethyl sulphides have shown characteristic patterns; in the ABC portion of an ABCX spin system (X = ¹⁹F) of the compounds, one of the subspectra shows an ABC pattern and the other apparently an AB₂ pattern. These spectral patterns have been analysed and the ¹H NMR data obtained are discussed briefly.     

Triphenylphosphine-Catalyzed Stereoselective Synthesis of Alkyl 3-(2-Naphthylsulfanyl)-2-propenoate from Alkyl Acetylenecarboxylates and 2-Naphthalenethiol

Protonation of the highly reactive 1:1 intermediates, produced in the reaction between triphenylphosphine and alkyl acetylenecarboxylates by 2-naphthalenethiol, leads to vinyltriphenylphosphonium salts, which undergo an addition–elimination reaction to produce the corresponding S-vinyl thioethers. The NMR spectra indicated that the compounds contained two stereoisomers for each S-vinyl thioether; their ratio was determined on the basis of ¹ H NMR spectra. The reaction is fairly stereoselective.     

2-（1H-咪唑-1-基）-1-（2，3，4-三甲氧基）苯乙酮肟酯新化合物合成与生物活性研究

首次合成了12个2-（1H-咪唑-1-基）-1-（2，3，4-三甲氧基）苯乙酮肟酯新 化合物，并经元素分析、红外光谱、核磁共振氢谱对其结构进行了表征，初步生物 活性测试表明，有些化合物具有杀菌活性。研究了这些新化合物结构与光谱特征之 间的关系。     

2-芳基-5-(4-硝基苯甲酰氨基)-1,3,4-噻二唑的合成

以芳甲酰肼和对硝基苯甲酰氯为主要原料, 合成出了10个酰氨基硫脲化合物5a～5j, 其中有6个(5d, 5f～5j)为新化合物. 在无需任何酸性催化剂条件下, 将制得的酰氨基硫脲在DMF中加热回流直接脱水关环合成出了9个2-芳基-5-(4-硝基苯甲酰氨基)-1,3,4-噻二唑化合物6a～6i, 其中7个(6b～6d, 6f～6i)为新化合物. 利用IR和1H NMR证明了化合物5存在两种异构体. 目标产物的结构通过IR, 1H NMR和元素分析进行了表征.     

19F and 1H NMR spectra of halocarbons

19F NMR chemical shifts and coupling constants are reported for 215 compounds. For 77 of these compounds, 1H NMR spectral data are also given. Long-range couplings, including 8J(F,F) and 5J(F,H), are reported. The complexity of halocarbon spectra owing to the presence of rotational isomers, asymmetric centers, long-range couplings, and chlorine isotope effects are illustrated, and the methods used for analyzing such complex spectra are briefly discussed.