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41.
Dina Moustafa Chelsea Sweet Hyun Lim Brenda Calalpa Parminder Kaur 《Tetrahedron letters》2018,59(42):3816-3820
A direct and efficient synthesis of arylketones via arylboronic acid addition to nitriles in presence of inexpensive Mn/Cu catalytic system is reported. The use of non-precious Mn and Cu salts has been found to be highly advantageous both in terms of accessibility as well as cost effectiveness. A series of arylboronic acids as well as nitriles were used to synthesize a variety of symmetrical and unsymmetrical arylketones. Based on the literature studies, the reaction mechanism is anticipated to go through an aryl radical intermediate which reacted with the copper activated nitrile to give the desired arylketones after the hydrolysis of the imine intermediate. 相似文献
42.
The synthesis of 1H-indazoles is achieved from o-aminobenzoximes by the selective activation of the oxime in the presence of the amino group. The reaction occurs with a variety of substituted o-aminobenzoximes using a slight excess of methanesulfonyl chloride and triethylamine at 0-23 degrees C and is amenable to scale-up. The synthesis of 1H-indazoles under these conditions is extremely mild compared with previous synthetic approaches and affords the desired compounds in good to excellent yields. 相似文献
43.
Ley SV Abad-Somovilla A Anderson JC Ayats C Bänteli R Beckmann E Boyer A Brasca MG Brice A Broughton HB Burke BJ Cleator E Craig D Denholm AA Denton RM Durand-Reville T Gobbi LB Göbel M Gray BL Grossmann RB Gutteridge CE Hahn N Harding SL Jennens DC Jennens L Lovell PJ Lovell HJ de la Puente ML Kolb HC Koot WJ Maslen SL McCusker CF Mattes A Pape AR Pinto A Santafianos D Scott JS Smith SC Somers AQ Spilling CD Stelzer F Toogood PL Turner RM Veitch GE Wood A Zumbrunn C 《Chemistry (Weinheim an der Bergstrasse, Germany)》2008,14(34):10683-10704
We describe in full the first synthesis of the potent insect antifeedant azadirachtin through a highly convergent approach. An O-alkylation reaction is used to unite decalin ketone and propargylic mesylate fragments, after which a Claisen rearrangement constructs the central C8-C14 bond in a stereoselective fashion. The allene which results from this sequence then enables a second critical carbon-carbon bond forming event whereby the [3.2.1] bicyclic system, present in the natural product, is generated via a 5-exo-radical cyclisation process. Finally, using knowledge gained through our early studies into the reactivity of the natural product, a series of carefully designed steps completes the synthesis of this challenging molecule. 相似文献
44.
45.
极化中子衍射方法常用于研究含未配对电子化合物中电子自旋密度的分布.分子中电子自旋密度分布从一个独特的角度反映化合物的磁性质.本文介绍极化中子衍射方法的背景知识和基本原理.包括中子源、中子和X射线衍射、极化中子衍射,以及一些常用的实验数据处理方法.选用几个实例总结了用极化中子衍射方法得到的电子自旋密度分布在无机和有机化学中的应用.通过单分子磁体[Fe8O2(OH)12(tacn)6]^8+和氰基桥联化合物K2[Mn(H2O)2]3[Mo(CN)7]2·6H2O,说明如何用该方法研究金属原子间的磁相互作用;并通过Ru(acac)3这个只含一个未配对电子的化合物来说明如何获得化合物中金属和配体上小的自旋密度;最后介绍了该方法在nitronylnitroxide自由基研究中的应用. 相似文献
46.
In this study, a capillary electrochromatography (CEC) method coupled either with UV or mass spectrometric detection was developed for the detection of trace-amounts of melamine and its related by-products (ammeline, ammelide, and cyanuric acid). A series of poly(divinyl benzene-alkene-vinylbenzyl trimethylammonium chloride) monolithic columns, which were prepared by a simple in situ polymerization with divinyl benzene (DVB), vinylbenzyl trimethylammonium chloride (VBTA) and different types of alkene monomers such as 1-octene, 1-dodecene or 1-octadecene were used as separation columns, with the poly(DVB-1-dodecene-VBTA) monolith as the optimal chromatographic material because it provided a better separation. The detection limits of four melamine derivatives were in the ranged of 0.6–2.18 mg L−1 by the optimal CEC–UV mode, and were reduced from 2.2 to 19.4 μg L−1 by the optimal CEC–MS mode. Finally, the proposed CEC methods successfully determined melamine contaminations (0.1 mg L−1 per analyte) in several dairy products as test samples with analyte recovery range of 69–85% (intra-day) and 68–75% (inter-day), and with peak area reproducibility range of 4.3–8.6% and 8.7–15.6% for intra-day and inter-day, respectively. This is the first report for CEC separation coupled with MS detection applied in trace melamine residue analyses with a faster separation and comparable or even better detection ability than previous GC–MS, CE–MS, as well as LC–MS methods. 相似文献
47.
Wan‐Ling Liu Yi‐Fen Hsu Yu‐Wei Liu Brenda Singco Ssu‐Wei Chen Hsi‐Ya Huang Ting‐Yu Chin 《Electrophoresis》2012,33(19-20):3008-3011
In this study, a rapid and sensitive method is described for the catecholamines detection in rat brain. CE with LIF detection for the determination of FITC derivatized catecholamines (dopamine, epinephrine, and norepinephrine) was demonstrated. Conventional water bath and microwave‐assisted derivatization methods were employed and a significant reduction in the derivatization time from 2 h for the conventional water bath at room temperature (ca. 25°C) to 2 min for the microwave‐assisted derivatization was achieved. Online sample concentration of field‐amplified sample stacking (FASS) method was employed to achieve higher sensitivities (the detection limits obtained in the normal injection mode ranged from 2.6 to 4.5 ng L?1 and in the FASS mode ranged from 22 to 34 pg L?1). Furthermore, this microwave‐assisted derivatization CE–LIF method successfully determined catecholamines in rat brain with as low as 100 ng L?1 (FASS mode) to 10 μg L?1 (normal injection mode). This CE–LIF method provided better detection ability when compared to the best reports on catecholamines analyses. 相似文献
48.
Muñoz MA Urzúa A Echeverría J Modak B Joseph-Nathan P 《Natural product communications》2011,6(6):759-762
Careful reevaluation of the 1H and 13C NMR spectroscopic data of filifolinol acetate (4) led to the reassignment of the C-10 and C-11 signals, as well as the gem-dimethyl signals. Single crystal X-ray analysis provided an independent structural confirmation of 4, and comparison of the experimental vibrational circular dichroism spectrum with calculations performed using density functional theory provided the absolute configuration of this 3H-spiro-1-benzofuran-2,1'-cyclohexane and related molecules. 相似文献
49.
Kanda S. Ramasamy Farid Bakir Brenda Baker P. Dan Cook 《Journal of heterocyclic chemistry》1993,30(5):1373-1377
The synthesis of benzylated N2-(4,7,10,13-tetraazatridec-1-yl)-2′-deoxyguanosines 4 was accomplished by a key nucleophilic reaction of the novel unsymmetrical polyamine 2 , with 3′,5′-O-(tetraisopropyldisiloxane-1,3-diyl)-2-chloro-2′-deoxyinosine ( 1 ). 相似文献
50.
Saldanha Renata Leal Gomes Bhetina Cunha da Rocha Torres Gabriel de Lima Brenda Raffaela de Castro José Adilson da Silva Ladário Ferreira Elivelton Alves 《Journal of Solid State Electrochemistry》2020,24(8):1991-1998
Journal of Solid State Electrochemistry - The anodic oxide on titanium can be thickened by anodization, with the consequent corrosion properties of this oxide depending on many variables, including... 相似文献