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791.
The reaction of 1-aryl-2-(dimethylaminomethylene)butane-1,3-diones with diethyl oxalate in the presence of sodium hydride in THF gave ethyl 5-aroyl-4-oxo-4H-pyran-2-carboxylates, from which 4-oxo-6-aryl-4H-pyran-2-carboxylic acids (6-arylcomanic acids) were obtained in high yields via acid-catalyzed deformylative rearrangement. 5-Aroyl-4-oxo-4H-pyran-2-carboxylic acids (5-aroylcomanic acids) were prepared via а ring-opening/ring-closure sequence by the reaction of 5-aroyl-2-carbethoxy-4-pyrones with piperidine and subsequent basic hydrolysis and acidification. 相似文献
792.
seco-Iso-cyclopropylfurano[e]indoline-trimethoxyindole 1 and seco-cyclopropylfurano[f]quinoline-trimethoxyindole 2 are potent cytotoxic agents. Previous synthesis of these compounds was inefficient and the approach required separation of a mixture containing the isomeric indoline and quinoline intermediates 11 and 12, formed from radical cyclization of allylic bromide 10. Reported herein is an efficient and selective synthesis of either intermediate 11 or 12, thus product 1 or 2, as needed. The conditions of the Stobbe condensation, bromination, 5-exo-trig radical cyclization, amine-carboxylic acid coupling, and debenzylation were optimized for multi gram scale. As a result, the reaction times were shortened, the products were readily isolated, and the yields and purity improved. 相似文献
793.
Sheng‐Run Zheng Xi‐Ling Wen Zi‐Meng Liu Tao Xie Jing‐Bo Tan Jun Fan Shuang‐Shuang Hou Wei‐Guang Zhang 《无机化学与普通化学杂志》2014,640(10):2057-2061
Two coordination polymers (CPs), namely, [Cu(Hptz)2(Hhba)2]n ( 1 ) [Hptz = 5‐(4‐pyridyl)‐1H‐tetrazole, H2hba = 2‐hydroxybenzoic acid] and [Zn3(ptz)2(hpa)2]n ( 2 ) (H2hpa = 2‐hydroxy‐2‐phenylacetic acid), were synthesized by solvothermal reactions. Both complexes were characterized by elemental analysis, infrared spectroscopy, powder X‐ray diffraction, thermogravimetric analysis, and single‐crystal X‐ray diffraction analysis. Compound 1 exhibits a 2D (4,4) network, where each layer connects to four adjacent layers to construct a 3D supramolecular framework. Compound 2 has a 3D framework structure composed of 1D SUBs, which are formed by both carboxyl and tetrazole groups. The complexes represent two rare examples of CPs constructed from Hptz and organic carboxyl acid ligands. Complex 2 exhibits intense, red‐shifted emissions in the visible region at room temperature. 相似文献
794.
Qun Dang Zhibo Zhang Bingyu Tang Yang Song Ling Wu Tongqian Chen Stephane Bogen Vinay Girijavallabhan David B. Olsen Peter T. Meinke 《Tetrahedron letters》2014
To discover novel nucleosides as potential antiviral agents, 2′-spirolactam and 2′-spiropyrrolidine-containing nucleoside analogs were envisioned. Efficient synthetic routes were developed with an epoxide opening as the key step to establish the quaternary center at the 2′ position, leading to the design and synthesis of uridine analogs 8 and 21, prodrugs 13–16, and cytidine analog 11. 相似文献
795.
Jabbar Khalafy Nasser EtivandShadi Dilmaghani Mahnaz EzzatiAhmad Poursattar Marjani 《Tetrahedron letters》2014
A simple and convenient synthesis of 2-aryl-3-hydroxy-6,7-dihydro-1H-indol-4(5H)-ones is achieved in high yields via the one-pot, three-component reaction of arylglyoxals, 1,3-cyclohexanedione, and ammonium acetate in water under reflux conditions. 相似文献
796.
A concise, two-step eco-friendly approach towards the synthesis of 5-sulfenyl tetrazole derivatives of indoles and pyrroles, is reported. The synthesis comprises the oxone-mediated thiocyanation of the starting heterocycles towards intermediate 3-thiocyanato indoles and 2-thiocyanato pyrroles, and their subsequent treatment with sodium azide in 2-propanol/water under zinc bromide promotion. 相似文献
797.
An efficient one-step method has been developed to construct furans via a Suzuki–Miyaura cross-coupling reaction of 1,2-oxaborol-2(5H)-ols with carboxylic anhydrides. In the presence of Pd(OAc)2/PCy3, the multi-substituted alkenylboron compounds could couple with anhydrides to obtain furans in moderate-to-good yields. The addition of bases promoted the coupling reaction, and the plausible reaction mechanism was proposed. 相似文献
798.
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
799.
含硼杂原子Na-B-ZSM-5分子筛对甲醇脱氢制甲醛反应的催化性能 总被引:1,自引:0,他引:1
以白炭黑为硅源、硼酸为硼源、NaOH为碱源、四丙基溴化铵(TPABr)和1,6-己二胺(HMDA)混合模板剂,采用水热合成法制备含硼杂原子Na-B-ZSM-5分子筛,用XRD、SEM、FT-IR、UV-vis、11B MAS NMR、NH3-TPD等方法对其进行表征。在连续流动常压固定床反应器上评价Na-B-ZSM-5分子筛对甲醇脱氢制甲醛反应的催化性能,考察n(Si)/n(B)、n(Na2O)/n(SiO2)、晶化温度和晶化时间等制备参数以及反应温度和质量空速等工艺参数对催化性能的影响。结果表明,硼进入了分子筛的骨架结构中,存在与B酸中心有关的骨架四配位硼和与L酸中心有关的骨架三配位硼,Na-B-ZSM-5分子筛含有较多的弱酸位和少量的中强酸位。催化剂的最佳制备参数为n(Si)/n(B)比值为7.5、n(Na2O)/n(SiO2)比值为0.14、晶化温度170℃、晶化时间48 h。Na-B-ZSM-5(7.5)分子筛在反应温度550℃、质量空速1.85 h-1的反应条件下对甲醇的转化率为62.97%,甲醛的选择性为68.86%。 相似文献
800.
采用两步晶化法制备ZSM-5/MCM-48微介孔复合分子筛,通过调变前驱体溶胶的晶化时间获得不同结构的ZSM-5/MCM-48基分子筛催化剂。采用XRD、N2-吸附、SEM、TEM、FT-IR和Py-FTIR等手段进行表征,结果表明,前驱体溶胶的晶化时间对ZSM-5/MCM-48复合分子筛的结构和表面酸性产生重要的影响,而特定结构的复合分子筛基催化剂可以显著改变甲醇制汽油(MTG)反应的产物分布,与ZSM-5基催化剂相比显著降低了油品中芳烃和均四甲苯的含量。阐明了其催化作用机制是由于介孔结构的MCM-48对微孔结构的ZSM-5界面或表面的修饰作用。 相似文献