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1.
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. 相似文献
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Treatment of 4-amino-3-(1-aryl-5-methyl-1,2,3-triazol-4-yl)-5-mercapto-1,2,4-triazoles/2-amino-5-(1-aryl-5-methyl-1,2,3-triazole-4-yl)-1,3,4-thiadiazoles with benzaldehyde,acetone and ω-bromoacetophenone was tested and compared.The title compounds Schiff bases,amides,imidazolo [2,1-b]-1,3,4-thiadiazoles and 7H-s-triazolo[3,4-b]-1,3,4-thiadiazines have been confirmed by elemental analyses,^1H NMR,IR and MS spectra.All the compounds have also been screened for their antibacterial activities against B.subtilis,S.aureus and E.coli. 相似文献
3.
The structures of five metabolites (2-6) of agarofuran 1 were confirmed by synthesis. The configuration of the secondary hydroxyl in 7 was determined by Horeau′s method. The configuration of C-2 in compound 4 and 5 was determined by their stereochemistry and NMR. 相似文献
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Thirteen new 2-alkylaminoimidazolones(4) wre rapidly synthesized by a new solution-phase parallel synthetic method,which includes aza-Wittig reaction of iminophosphorane(1) with aromatic isocyanate to give carbodi-imide(2) and subsequent reaction of 2 with various aliphatic primary amine in a parallel fashion.The products were confirmed by ^1H NMR,MS,IR and X-ray crystallographic analysis.The unusual selectivity of the cyclization was probably due to the deometry of the guanidine intermediate. 相似文献
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A New Technique of Synthesizing 10—Hydroxy—5—methyl—5,10—dihydrophenophosphazine 10—Oxide 总被引:1,自引:0,他引:1
ZhiGangYIN DeFengZHAO 《中国化学快报》2003,14(4):347-350
10-Hydroxy-5-methyl-5,10-dihydrophenophosphazine 10-oxide(1)was prepared by a new technique of treating 10-methoxy-5,10-dihydrophenophosphazine 10-oxide(2)with an equivalent of NaH in anhydrous DMF,and then at 120℃ for 3-4h,which not only avoided poisonous and expensive methyl iodide used in literature,but made the consumption of NaH greatly decrease as well.The possible reaction mechanism was also described.The chemical structure of 1 was confiremed by IR,NMR,and mass spectroscopy. 相似文献
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The syntheses of three new optically active β-mercaptoalcohols,(R)-1,1-diphenyl-2-mercapto-3-methyl-1-butanol,(R)-1,1-diphenyl-2-mercapto-4-methyl-1-pentanol,and (R)-1,1-diphenyl-2-mercapto-1-benzenepropanol from the corresponding amino acids are described.The enantiomeric excesses of these β-mercaptoalcohols were determined by ^1H NMR as their (S)-mandeloyl derivatives. 相似文献
7.
For the first time the isomerization of 1,3,2-diazaphospholidine-2-sclenide dervatives in refluxing benzene in the presence of trace water was observed. The structures of isomerized products were determined by IR, ^1H NMR,^31P NMR, elemental analysis and X-ray crystallography. The mechanism of isomerization was also proposed. 相似文献
8.
Synthesis,Crystal Structure of Cis—dioxo—catecholatotungsten(VI) Complex and Its NMR Studies on the Interaction with ATP 总被引:1,自引:0,他引:1
Cis-dioxo-catecholatotungsten(VI) complex anion[W^(VI)O2-(OC6H4O)2]^2- was obtained with discrete protonated ethylenediamine (NH2CH2CH2NH3)^ cations by the reaction of tetrabutyl ammonium decatungstate with catechol in the mixed solvent of CH3OH,CH3CN and ethylenediamine,and compared with its molybdenum anaogue [Mo^(V) O2(OC6H4O)2]^3- by crystal structure,UV,EPR,The results of the UV and EPR spectra show that tungsten is less redox active than molybdenum since the molybdenum is reduced from Mo(VI) to Mo(V) but tungsten stays in the original highest oxidized state Mo(VI) when they are crystallized from the solution above.It is worthy to note that [W^(VI)O2(OC6H4O)]^2- shows the same coordination structure as its molybdenum analogue in which the metal center exhibits distorted octahedral coordination geometry with two cis-dioxocatecholate ligands and might have the related coordination structure feature with the cofactor of flavoenzyme because [Mo^(V)O2(OC6H4O)2]^3- presented essentially the same EPR spectra as flavoenzyme.The NMR studies on the interaction of the title complex with ATP reveal that the reduction of W(VI) to W(V) occurs when the title complex is dissolved in D2O and the W(V) is oxidized again when ATP solution is mixed with original solution and the hydrolysis of the catecholato ligand take places at mean time being monitored by ^1H NMR and ^13C NMR spectra. 相似文献
9.
Several isoxazoline compounds were obtained by the 1,3-dipolar cycloaddition of benzonitrile oxide to 5-(R)-(1-menthyloxy)-2(5H)-furanone. The reaction condition was investigated preliminarily, the structures of these compounds have been established via the analysis of NMR data (involved NOEID or HMBC) and the reaction seems occurred regioselectively. 相似文献
10.
A new method for synthesis of 3-azido-3-deoxyxylofuranoside was described. D-ribose was methylated, then treated with methanesulfonyl chloride to give Ⅱ.Ⅱ was selectively replaced by benzoate at the 5-position to give Ⅲ. All these processes gave good yields. Ⅲ was treated with sodium azide to afford Ⅳ, whose structure was determined by ^1H NMR and ^13C NMR. 相似文献
11.
以D-葡萄糖为原料,经碳苷化反应,酰化反应和脯氨酸-DIPEA催化的aldol反应制得2个碳苷糖[1-(4'-羟基苯基)-4-C-β-四乙酰基葡萄糖基-3-烯-2-酮(5a)和1-(3-羟基苯基)-4-C-β-四乙酰基葡萄糖基-3-烯-2-酮(5b)];5与琥珀酸维生素D2经Steglich酯化反应合成了2个新型碳苷糖类维生素D2衍生物,其结构经1H NMR,13C NMR和HR-ESI-MS表征。 相似文献
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以N-羟基-4-甲氧基苯甲醛肟氯化物为原料,经两步反应制得3-对甲氧基苯基-5-甲基-异噁唑-4-甲酰肼(3);3依次经缩合和环合反应合成了一系列新型的2-芳基3-乙酰基-5-(3-对甲氧基苯基-5-甲基-异噁唑-4-基)-Δ4-1,3,4-噁二唑啉衍生物,其结构经~1H NMR,13C NMR,IR,MS(EI)和元素分析表征。 相似文献
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以(S)-2-氨基丙醇和氯乙酰氯为起始原料,经酰化和环合反应制得(S)-5-甲基吗啉-3-酮(4); 4经还原制得(S)-3-甲基吗啉(5); 5与4-溴-2-甲基苯甲酸酰化缩合合成了(S)-(4-溴2-甲基苯基)(3-甲基吗啉)-甲酮,总收率57%,其结构经1H NMR 和 13C NMR确证。 相似文献
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Katritzky AR Akhmedov NG Wang M Rostek CJ Steel PJ 《Magnetic resonance in chemistry : MRC》2004,42(7):648-658
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. 相似文献
19.
以2-氰基-6-羟基苯并噻唑为原料,与溴乙醛缩二乙醇缩合制得缩醛后再水解合成中间体6-(2-羰乙基)苯并[d]噻唑-2-甲腈(2);7-苯乙酰氨基-3-氯甲基头孢菌烷酸二苯甲酯依次经碘代和Wittig反应得(Z)-3-[3-(2-氰基苯并[d]噻唑-6-氧)丙-1-烯]-8-羰基-7-(2-苯乙酰氨基)-5-噻-1-氮[4.2.0]辛-2-烯-2-甲酸二苯甲酯(5);5经脱保护、缩合和氧化反应合成了3个新的Bluco类似物,其结构经1H NMR,13C NMR和HR-MS(ESI)表征。 相似文献
20.
Siva Lakshmi Devi A Srinivasa Rao Y Suresh Y Yogeswar Reddy M Jyothi G Rajababu B Prasad VS Umamaheswar Rao V 《Magnetic resonance in chemistry : MRC》2007,45(5):424-429
We report the complete (1)H and (13)C NMR assignment of impurities of six Lopinavir (2S)-N-[(2S, 4S, 5S)-5-{[2-(2,6-dimethylphenoxy)acetyl]amino}-4-hydroxy-1,6-diphenyl hexan-2-yl]-3-methyl-2-(2-oxo-1,3-diazinan-1-yl)butan- amide. Two of the impurities are regioisomers and GCOSY used to differentiate the two structures. The spectral assignments for all six impurities were achieved by concerted application of one and two-dimensional NMR techniques ((1)H NMR, (13)C NMR, DEPT, GCOSY, GHSQC and GHMBC). 相似文献