碲氢化钠存在下3－氧代硫代羧酸酯的一步合成法

３－氧代硫代羧酸酯可由α－溴代酮与碲氢化钠作用形成的烯醇盐与二硫代碳酸二乙酯进行乙氧硫代羰基化反应制得。３－氧代硫代羧酸酯的烯醇含量可由核磁共振谱测得     

Synthesis of 2-thioxo-1,3-thiazolidin-4-one derivatives

A series of new 2-thioxo-1,3-thiazolidin-4-one derivatives containing arylidene, arylazo, and aminomethylene fragments in position 5 of the rhodanine cycle was synthesized. Dedicated to Academician V. A. Tartakovsky on the occasion of his 75th birthday. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1564–1569, August, 2007.     

Synthesis and structure of 4-arylspirodihydro-pyranochromen-2-one derivatives

Syntheses are reported for sulfur-and nitrogen-containing derivatives of 4-arylspiro-2-benzopyranones modified at the exocyclic oxygen atom. The structure of these products was demonstrated by correlational NMR spectroscopy. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 518–527, April, 2007.     

Novel Synthesis of Condensed Pyridin-2(1H)-one and Pyrimidine Derivatives

The reaction of N-chloroacetyl derivatives 6-10 with morpholine yielded N-morpholin-1-yl acetyl derivatives 11-15 , which were subjected to Thorpe-Zieler cyclization with sodium tert -butoxide to produce the corresponding condensed pyridin-2(1H)-one derivatives 16-20 . Treatment of compounds 1 , 6-10 with either malononitrile or p -chlorobenzylidinemalononitrile in presence of triethylamine, afforded the corresponding pyrimidines 21-25 , 27 and pyridine derivative 26 respectively. Moreover compound 1 a was treated with ethyl isothiocyanoacetate to give the corresponding piprazine derivative 28 .     

One-Pot Synthesis of 4-Hydroxy-3-phenyl-2H-pyrano[3,2-b]benzofuran-2-one Derivatives

Novel 4-hydroxy-3-phenyl-2H-pyrano[3,2-b]benzofuran-2-ones (15a–d), were synthesized in a one-step procedure by the reaction of substituted benzofuran-3-ones 12a–d and (chlorocarbonyl)phenyl ketene.     

2,5-二吡唑基-1,3,4-噁二唑的一锅煮法合成及生物活性

１,３,４－二唑类化合物具有广泛的生物生理活性,如杀菌［１］、除草［２］、杀虫［３］和消炎［４］等,而２,５－二芳基－１,３,４－二唑类化合物一般具有昆虫生长调节活性,１９８０年美国Ｄｏｗ公司报道了２,５－双（２,４－二氯苯基）－１,３,４－二...     

Synthesis of Novel Piperazine Phosphoramidate Analogues of 2-Arylquinolones

A series of novel piperazine phosphoramidate derivatives of 2-arylquinolones were synthesized to improve their physicochemical and biological properties through a facile phosphorylating reaction. Their structures were elucidated by NMR, ESI MS, and HRMS.     

新型螺{二氢吲哚-3,2'-[1,3,4]噁二唑}-2-酮类似物的合成

靛红及其衍生物与丙二腈缩合得中间体2-(2-氧代吲哚-3-叉基)丙二腈及其衍生物(2l~2t);苯甲酸及其衍生物与水合肼缩合得苯甲酰肼及其衍生物(4a~4l);2和4分别经环合反应合成了20个螺{二氢吲哚-3,2'-[1,3,4]噁二唑}-2-酮类似物(5a~5t),其中5b~5t为新化合物,其结构经1H NMR和ESI-MS表征。     

5-芳酰氨基-2-苯基-2H-1, 2, 4-噻二唑-3-酮的合成

用1-芳酰基-5-苯基-2-硫代双脲与溴进行氧化成环反应制备了九个新的5-芳酰氨基-2-苯基-2H-1, 2, 4-噻二唑-3-酮, 相应的1-芳酰基-5-苯基-2-硫代双脲可以通过苯基脲与酰基异硫氰酸酯加成制得。     

One‐Pot Synthesis of CdSe Quantum Dots in Aqueous Solution for Biological Labeling

The one‐pot synthesis of water‐soluble and biologically compatible yellow CdSe quantum dots (QDs) featuring the use of glutathione (GSH) as the capping and reducing agent was achieved under aqueous conditions at 150 °C. The synthesized yellow CdSe QDs with quantum yield (QY) up to 20% exhibit zinc blende cubic structure particles with an average diameter of 4‐5 nm. It was found that both molar ratio of Se/Cd and reaction time had a significant effect on size distribution of GSH‐CdSe QDs. Meanwhile, the interaction of QDs bioconjugated to bovine hemoglobin (BHb) was studied by absorption and fluorescence(FL) spectra. With addition of BHb, the FL intensity of CdSe QDs largely quenched due to the static mechanism. The linear range is 5.0 × 10^?8 mol/L to 3.0 × 10^?6 mol/L, and the correlation coefficient is 0.9991, suggesting that could be used as a probe to label biological molecules and bacterial cells.     

Synthesis and Vasodilatory Activities of New Pyrazolo[3,4—d] pyrimidin—4—one Derivatives

A series of pyrazole[3,4-d] pyrimidin-4-one derivatives were synthesized and tested for vasodilatory activities. All of them were new compounds and their structures were confirmed by IR,^1H NMR,MS and elemental analysis.     

Synthesis of Asymmetric Propanetriol Analogues

Form natural tartaric acid,(R)-2-benzyloxy-3-(2-tertrahydropyranyloxy) propanol 3 was designed and synthesized, and (R)-2-benzyloxy-3-(4-methoxybenzyloxy)propanol 7 was prepared in a new method. They can be used as chiral synthons of lysophosphatidic acid and other compounds with asymmetric propanetriol backbone.     

Synthesis and Biological Evaluation of Pyranone Analogues of Territrem B

As a highly selective and potent acetylcholinesterase(AChE)inhibitor,territrem B wasisolated by Ling et al.from a strain of Aspergillus terreus in19791,2.Zhao et alreported mimic preparation of territrem B analogues from triterpenoids and found thatthe enone moiety and aromatic ring played important roles in their syntheticcompounds3,4.To further detect essential pharmacophors for AChE inhibitors,wesimplified the A/B ring system of territrem B and synthesized a number of pyranonepharmacop…     

Synthesis and Structure of Ethyl 3-acetamido-4-aryl-6-methyl-2-oxo-3,4-dihydropyran-5-carboxylates

Two ethyl 3-acetamido-4-aryl-6-methyl-2-oxo-3,4-dihydropyran-5-carboxylates(3) were synthesized with high diastereoselectivities and characterized by IR,NMR and MS.The configuration of 3a was confirmed by single-crystal X-ray diffraction,ethyl 3-acetamido-4-(4-nitrophenyl)-6-methyl-2-oxo-3,4-dihydropyran-5-carboxylate(3a),C17H18N2O7.The crystal is of orthorhombic,space group Pbca with a = 11.7781(16),b = 9.5979(10),c = 32.115(3),V = 3630.4(7)3,Z = 8,Mr = 362.33,Dc = 1.326 Mg/m3,λ = 0.71073,μ(MoKα) = 0.104 mm-1,F(000) = 1520,the final R = 0.0646 and wR = 0.1464 for 1788 observed reflections with I > 2σ(I).The N-H and oxygen atom are involved in intermolecular hydrogen bonds which link the molecules into a one-dimensional chain and stabilize the structure.     

Green synthesis of 3,4-dihydropyrimidinones using nano Fe3O4@meglumine sulfonic acid as a new efficient solid acid catalyst under microwave irradiation

Design, synthesis and characterization of nano Fe₃O₄@meglumine sulfonic acid as a new solid acid catalyst for the simple and green one pot multicomponent synthesis of 3,4-dihydropyrimidin-2(1H)-ones/thiones was studied. New solid acid catalyst was prepared through a clean and simple protocol and characterized using FTIR, VSM, TGA, SEM, elemental analysis (CHN) and XRD techniques. Heterogenization of homogeneous catalyst as a green approach is a useful method for enhancing the efficiency of catalyst. Presented study was a new method for attachment of homogeneous highly soluble catalyst (meglumine sulfate) to the magnetite nanoparticle surfaces for preparing a heterogeneous and effective catalyst. Obtained heterogeneous and reusable solid acid catalyst has high performance in the synthesis of Biginelli compounds. The reaction was performed under microwave irradiation as a rapid and green condition. Easy work up as well as excellent yield (90–98%) of products in short reaction times (40–200 s) and reusable catalyst are the main advantages of presented procedure. Reaction products were characterized in details using physical and chemical techniques such as melting point, ¹H NMR, ¹³C NMR and FTIR.     

Synthesis of 4-Pyridyl-2,3-dihydro-1H-1,5-benzodiazepin-2-ones

4-Pyridyl-2,3-dihydro-1H-1,5-benzodiazepin-2-ones were obtained by the condensation of ethyl nicotinoyl- or isonicotinoylacetates with o-phenylenediamine. Alkylation of the pyridylbenzodiazepinones with ethyl iodide under phase-transfer catalysis conditions occurred at the amide nitrogen of the heterocycle, whereas in nitromethane it occurred at the nitrogen of the pyridine substituent. Bromination with N-bromosuccinimide occurred at position 3 of the heterocycle. Pyridyldibenzodiazepinones underwent thermal rearrangement to derivatives of vinylbenzimidazole.     

6-氯-2(1 H)-喹喔酮合成方法的改进

设计了以对氯苯胺和氯乙酰氯为原料,经缩合、硝化、还原、环合、氧化五步制得6-氯-2(1H)-喹喔酮的位置选择性合成方法,并对以氯乙酰氯作为苯胺的氨基保护试剂进行硝化的反应和对含活泼氯的硝基化合物进行还原的反应进行了研究.研究结果表明以氯乙酰氯作为苯胺的氨基保护试剂进行硝化的反应符合一般的硝化定位规则,而含活泼氯的硝基化合物的还原在优化条件下以铁粉为还原剂可以高选择性获得目标产物.     

Synthesis of a novel water-soluble polyamide dendrimer based on a facile convergent method

A novel, rapid, inexpensive, and highly efficient convergent approach has been developed for the synthesis of a 32-amine-terminated G3 polyamide dendrimer by the hydrolysis of the dendrimer with trifluoroacetamide groups. The resulting dendrimer could be successfully modified with oligo(ethylene glycol) chains at its periphery to afford a novel water-soluble polyamide dendrimer. The structural homogeneity of the dendrimers was confirmed by NMR and MALDI-TOF mass spectroscopies.     

Synthesis of new 3,3-dimethoxyazetidine-2-carboxylic acid derivatives

Cyclization of γ-amino-α-bromocarboxylic esters resulted in an efficient synthesis of new 3,3-dimethoxyazetidine-2-carboxylates, that is, methyl N-t-butyl-3,3-dimethoxyazetidine-2-carboxylic ester and 3,3-dimethoxyazetidine-2-carboxylic acid, or 3-bromo-4,4-dimethoxypyrrolidin-2-ones, depending on the substituent at nitrogen. Reduction of the 3,3-dimethoxyazetidine-2-carboxylates gave the corresponding 3,3-dimethoxy-2-(hydroxymethyl)azetidines. These novel cyclic amino acid derivatives, available on multigram scale, have a suitably protected carbonyl function at the 3-position, which enables further functionalization.     

西地那非类似物的合成

报道了一种合成西地那非类似物的新方法。以邻丙氧基苯甲酸为原料,经5步反应制得西地那非类似物的关键中间体--硫代西地那非氯{1-甲基-3-丙基-5-(2-丙氧基-5-氯磺酰苯基)-1,6-二氢-7H-吡唑并［4,3-d］嘧啶-7-硫酮}(7); 7与哌嗪衍生物反应合成了4个新型的西地那非类似物,收率72.3%~80.9%,纯度99.0%,其结构经¹H NMR和ESI-MS表征。