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961.
We report a highly efficient method for the synthesis of (Z)-3-ylidenephthalides via intramolecular cyclization of readily available 2-acyl-benzoic acids mediated by TSTU at room temperature. Using this method, diversely substituted (Z)-3-ylidenephthalides have been generated in good to excellent yields. The application of the method is highlighted by gram-scale preparation of the antiplatelet drug n-butylphthalide. 相似文献
962.
Transition-metal-catalyzed isoquinoline synthesis that profits from the strategy of chelation-assisted C−H activation has flourished over the past decade. By virtue of the directed C−H bond cleavage of imines, amines, amidines, oximes, hydroximoyl halides, hydrazones, or azines, diverse isoquinoline derivatives have been accessed from alkynes, conjugated dienes, or diazo compounds under the catalysis of rhodium, ruthenium, palladium, nickel, or manganese. This digest summarizes the annulation reactions via chelation-assisted C−H activation leading to isoquinolines, isoquinolinium salts, or isoquinoline N-oxides. 相似文献
963.
Hucheng Zhu Lijun Huan Chunmei Chen Jing Yang Jiangbo He Yong Chen Guangmin Yao Zengwei Luo Yongbo Xue Yonghui Zhang 《Tetrahedron letters》2014
A pair of unprecedented enantiomers (1a/1b) of cyclohexylethanoid bearing an unusual trioxabicyclo[4.2.1]nonane ring, along with two known structurally related cyclohexylethanoids, (+)-rengyolone (2) and cleroindicin E (3), were isolated from the aerial parts of Clerodendrum bungei. The structures and absolute configurations of the enantiomers were determined by comprehensive spectroscopic analysis, single-crystal X-ray diffraction, and quantum mechanical calculation of the electronic circular dichroic (ECD) spectra. The postulated biogenetic pathway of 1a/1b was also discussed. 相似文献
964.
α-Hydroxyallylphosphinates were stereoselectively converted to γ-chloro allylphosphinates when treated with Ph3P and CCl4, via substitution of hydroxyl and migration of double bond. The reaction was promoted by phosphonium cation that acted as Lewis acid. 相似文献
965.
Chao He Xiaohui Zhang Ruofeng Huang Jing Pan Jiaqiang Li Xuege Ling Yan Xiong Xiangming Zhu 《Tetrahedron letters》2014
Under open-flask conditions, an efficient method to assemble a series of diversely functionalized diarylketones in the presence of commercially available NBS has been developed. Yields of up to 99% have been achieved employing diarylmethanes as starting material. Based on 18O-labeled experiment, the addition of stoichiometric water eventually leads to excellent yields in all carbonylation cases. 相似文献
966.
Qun Dang Zhibo Zhang Shuangsheng He Yaohong Liu Tongqian Chen Stephane Bogen Vinay Girijavallabhan David B. Olsen Peter T. Meinke 《Tetrahedron letters》2014
To discover novel nucleosides as potential antiviral agents, 4′-spirocyclic phosphono-nucleosides were designed to mimic the monophosphate of R-1479, a known nucleoside inhibitor of HCV NS5B. Bypassing the first kinase step to nucleoside monophosphate is viewed as advantageous since this phosphorylation is often observed as the rate-limiting transformation to the active NTP for many nucleosides. Efficient synthetic routes were developed with a triphenylphosphine–iodine cyclization reaction as the key step to form the tetrahydrofuran 4′-spirocycle. The desired 4′-spirocyclic phosphono-cytidine analogs 12a, 12b, and 16 were prepared in 11 steps. 相似文献
967.
This article discusses the effect of water fraction on the rheological properties of waxy crude oil emulsions including gel point, yield stress, viscosity, and thixotropy. The experimental results reveal that the rheological behaviors of the w/o emulsion samples all intensify with the increase of water volume fraction within 60%. Of more significance is that a correlation for w/o emulsions between yield stress and water volume fraction is put forward with an average relative error of 6.75%. In addition, some mainstream viscosity prediction models of w/o emulsions are evaluated, and Elgibaly model is the best-fit for the emulsions in this study. 相似文献
968.
Yulin He Weina Zhou Xiangcheng Wang Baoliang Bao Guojian Zhang Cheng Wang Chunmei Wang Xuemei Wang Wei Fang 《Journal of Radioanalytical and Nuclear Chemistry》2014,301(2):469-474
In this study, we synthesized and characterized N-[11C]methyl-dopamine ([11C]MDA) for cardiac sympathetic nerve imaging. [11C]MDA was synthesized by direct N-methylation of dopamine with [11C]methyl iodide and purified by semi-preparation reverse high pressure liquid chromatography (HPLC). The total synthesis time was 45 min including HPLC purification. The radiochemical yields of [11C]MDA was 20 ± 3 %, without decay correction. The radiochemical purity was >98 % and the specific activity was about 50 GBq/mmol. The biological properties of [11C]MDA were evaluated by biodistribution study in normal mice. PET imaging was performed in healthy Chinese mini-swines. Biodistribution study showed that [11C]MDA had high myocardium uptake. PET/CT imaging showed [11C]MDA had clear and symmetrical myocardium uptake, which was blocked obviously by injecting imipramine hydrochloride. [11C]MDA would be a promising candidate of radiotracer for cardiac sympathetic nervous system imaging. 相似文献
969.
Xiao-gui Feng Qian-ge He Jian-chen Wang Jing Chen 《Journal of Radioanalytical and Nuclear Chemistry》2014,299(1):509-516
90Sr is a product of nuclear fission, the radioactivity of which can be determined by liquid scintillation counting (LSC). Because the LSC spectra of 90Sr and its daughter 90Y overlap each other, the following methods are usually used: (1) measuring immediately after 90Sr/90Y separation; (2) waiting to reach radioactive equilibrium; (3) adopting the conventional 2-window approach; and (4) using the spectra deconvolution technique. The first one requires 90Sr/90Y separation and immediate measurement; the second one is time-consuming; the third one is valid only for samples with the same quench level as the calibration standard; the last one is somewhat complicated, and in some cases it is not convenient to export the experimental data to some deconvolution software. Therefore, we have developed a modified 2-window approach to rapidly determine 90Sr and 90Y in either equilibrium or disequilibrium at low quench level. The key modification of the approach is to provide an LSC spectrum of pure 90Y with the same quench level as the sample to be determined. This modification eliminates the need to conduct 90Sr/90Y separation for the sample itself, to prepare the quench curves, and to fit the LSC spectra with some deconvolution software. 相似文献
970.
Peng He Xiaolin Hou Ala Aldahan Göran Possnert 《Journal of Radioanalytical and Nuclear Chemistry》2014,299(1):249-253
Relatively large amounts of radioactive iodine 129I (T 1/2 = 15.7 Ma) have been documented in seawater such as the English Channel, the Irish Sea and the North Sea. Data on the concentration of the iodine isotopes in waters of the Celtic Sea are missing. Aiming to provide first 129I data in the Celtic Sea and compare them with levels in the other close-by seawater bodies, surface seawater samples were analyzed for the determination of 127I and 129I concentrations. The results revealed a high level of 129I in these waters and suggest strong influence by liquid discharges from La Hague and Sellafield reprocessing facilities. 127I concentrations are rather constant while the 129I/127I ratio reaches up to 2.8 × 10?8 (ranging from 10?10 to 10?8), which is 2–4 orders of magnitude higher than pre-nuclear era natural level. Transport of 129I to the Celtic Sea is difficult to depict accurately since available data are sparse. Most likely, however, that discharges originated from La Hague may have more influence on the Celtic Sea 129I concentrations than the Sellafield. Comprehensive surface water and depth profiles 129I data will be needed in the future for assessment of environmental impact in the region. 相似文献