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21.
Iida T Satoh H Maeda K Yamamoto Y Asakawa K Sawada N Wada T Kadowaki C Itoh T Mase T Weissman SA Tschaen D Krska S Volante RP 《The Journal of organic chemistry》2005,70(23):9222-9229
[Reaction: see text]. The synthesis of neuropeptide Y antagonist 1, currently under clinical investigation for the treatment of obesity, is described. The convergent synthesis from trans-spirolactone carboxylic acid intermediate 2a and aminopyrazole 3 is predicated on a stereoselective route to the former. The coupling reaction of ethyl 4-oxocyclohexanecarboxylate (10a) with lithiated isonicotinamide 11 was investigated in detail, but even optimized conditions only provided a 45:55 ratio of trans:cis isomers (12a:12b). While selective crystallization schemes were developed to isolate the thermodynamically less stable trans isomer 2a, improved stereocontrol was subsequentially achieved by the application of ketene chemistry. The ketene formation and quench was investigated under a variety of conditions aimed at maximizing the trans:cis ratio. Reacting a mixture of carboxylic acids 2a and 2b with POCl3 in THF, followed by concomitant addition of tert-butyl alcohol in the presence of TMEDA at 35 degrees C provided a 4:1 ratio of trans:cis tert-butyl esters (18a:18b) via in situ ketene formation. Ester hydrolysis, followed by selective crystallization of undesired 2b as the HCl salt, led to isolation of 2a in 47% overall yield. Aminopyrazole intermediate 3 was synthesized via the condensation reaction of 2-fluorophenylhydrazine hydrochloride (4a) with acrylonitrile derivative 5 in 65-70% yield. Coupling of advanced intermediates 2a and 3b via activation with thionyl chloride gave a 92% yield of 1. 相似文献
22.
A number of 2-thioxopyrido[3′,2′:4,5]thieno[3,2-H]pyrimdin-4(3H-ones (5) have been synthesized by cyclocondensation of 2-carbethoxy-3-amino-4-phenyl-6-substituted-thieno[2,3-b]pyridines (3) with various isothiocyanates. Compounds 5 were S-methylated routinely and the reactions compared under solid-liquid phase transfer conditions to obtain 2-methylthiopyrido[3′,2′:4,5]thieno[3,2-d]pyrimidin-4(3H)-ones (6). The new triheterocyclic pyridothienopyrimidines were prepared with the objective to study their pharmacological properties. 相似文献
23.
Green synthesis and characterization of silver nanoparticles by Allium cepa L. to produce silver nano‐coated fabric and their antimicrobial evaluation
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Prashansa Sharma Suman Pant Shambhavi Rai Renu Bala Yadav Swapnil Sharma Vivek Dave 《应用有机金属化学》2018,32(3)
This research work was proposed to study the antimicrobial activity of the silver nanocoated fabric with the purpose of producing good dressing and clothing material. We synthesized simple, ecofriendly, cost‐effective and sustainable silver nanoparticles by using the aqueous extract of Allium cepa L. Here, A. cepa L. acts as a good reducing and capping agent that produced stable silver nanoparticles having particle size of range 36 ± 1 to 98 ± 2 nm, Poly dispersiblity index 0.234 ± 0.61 to 1.023 ± 0.33 and Zeta potential ‐12 ± 1.5 mV to ‐26 ± 1.2 mV. The effect of temperature and extract volume used was considered for optimization of synthetic procedure. The nanocoated fabric was characterized for morphological study, size (using transmission electron microscopy (TEM) and field emission scanning electron microscopy (FE‐SEM) and zeta‐potential (Zeta Potentiometer). The presence of functional groups were observed by using attenuated total reflection‐Fourier transform infrared (ATR‐FTIR) and Raman spectroscopy. The crystallinity and structural property of the synthesized silver nanoparticles were studied in terms of Powder X‐ray diffraction (PXRD). An IC50 value and zone of inhibition was studied which demonstrate that the silver nanocoated fabric have an excellent antibacterial property against Gram‐negative (Escherichia coli) and Gram‐positive (Staphylococcus aureus) bacteria. Further nanocoated fabric material was washed (with function of time 0, 10, 25, and 50 laundry cycles) and still retained their anti‐bacterial activity towards both strain. Initially there was 52 μg/ml of silver nanoparticles on the cotton fabric but after 50 laundry cycle in 500 ml of distilled water the fabric showed 92% efficiency against gram positive and 90% efficacy toward gram negative bacteria. It was found that 4.16 μg/ml nano particles leached in case of S. Aureus and 5.2 μg/mL silver nanoparticles leached in case of E. coli. Nanocoated fabric material synthesized using green synthesis was found to be economical with good resistance to washing. 相似文献
24.
We have synthesized a homologous series of azoesters consisting of a coumaryl moiety as the end group. Eleven derivatives of this series exhibit mesomorphism. The nematic mesophase is exhibited from ethyl homologue onward, while the smectic phase commences at the pentyl derivative and is exhibited along with the nematic phase up to the hexadecyl derivative. The N-I transition temperatures curves show the usual odd-even effect. All the compounds in this series are thermally stable and exhibit a wide mesomorphic range of nearly 120°C. Their thermal stabilities and other characteristics are discussed. 相似文献
25.
The oxidation of alkyl chlorides and bromides with dimethyl sulfoxide has been performed in the presence of sodium iodide. This method allows a convenient one-step procedure for the preparation of aldehydes from alkyl chlorides and bromides. 相似文献
26.
A recent communication1 in this journal reported the reaction of o-tolunitrile with sodium in tetrahydrofuran to yield a compound, m.p. 123.5–124°, to which was assigned the isoindole structure 1. A plausible mechanism can be written for the formation of 1 involving reductive dimerization of the cyano groups of two molecules of the nitrile, subsequent 1,5-hydrogen shift from a methyl group, disrotatory electrocyclic isoindole ring closure, and finally air oxidation and tautomerization to 1. Nevertheless, the evidence presented did not require an isoindole structure. Moreover, it would be unusual for a primary enamine to survive. 相似文献
27.
Matthew Wallace Andre Zamith Cardoso Dr. William J. Frith Dr. Jonathan A. Iggo Dr. Dave J. Adams 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(50):16484-16487
The magnetic‐field‐induced alignment of the fibrillar structures present in an aqueous solution of a dipeptide gelator, and the subsequent retention of this alignment upon transformation to a hydrogel upon the addition of CaCl2 or upon a reduction in solution pH is reported. Utilising the switchable nature of the magnetic field coupled with the slow diffusion of CaCl2, it is possible to precisely control the extent of anisotropy across a hydrogel, something that is generally very difficult to do using alternative methods. The approach is readily extended to other compounds that form viscous solutions at high pH. It is expected that this work will greatly expand the utility of such low‐molecular‐weight gelators (LMWG) in areas where alignment is key. 相似文献
28.
29.
Ganesh P. Sanganwar Ram B. Gupta Alexandre Ermoline James V. Scicolone Rajesh N. Dave 《Journal of nanoparticle research》2009,11(2):405-419
Due to the increased use of nanocomposites, mixing at nanoscale has become important. Current mixing techniques can be classified
into: (a) dry mixing (mechanical mixing), (b) wet mixing, and (c) simultaneous production of mixed nanoparticles (when possible).
Dry mixing is in general not effective in achieving desired mixing at nanoscale, whereas wet mixing suffers from different
disadvantages like nanomaterial of interest should be insoluble, has to wet the liquid, and involves additional steps of filtration
and drying. This paper examines the use of pressurized carbon dioxide having high density and low viscosity to replace the
liquids (e.g., n-hexane, toluene). Ultrasound is applied to the suspension of nanopowders in gaseous and supercritical carbon dioxide where
high impact collisions during sonication help mixing and the final mixture is obtained by simple depressurization. The method
is tested for binary mixture of alumina/silica, silica/titania, MWNT (multiwalled carbon nanotubes)/silica, and MWNT/titania.
The effects of sonication intensity and pressure on the degree of mixing are studied. Comparative study is also done with
liquid n-hexane as a mixing media. Quantitative characterization (e.g., mean composition standard deviation, intensity of segregation)
of mixing of alumina/silica and silica/titania is done with energy-dispersive X-ray spectroscopy, and that of MWNT/silica
and MWNT/titania is done using field-emission scanning electron microscopy and day-light illumination spectrophotometry. Results
show that mixing in carbon dioxide at higher ultrasound amplitudes is as good as in liquid n-hexane, and the final mixed product does not contain any residual media as in the case of liquid n-hexane. 相似文献
30.
Derk Brouwer Birgit van Duuren-Stuurman Markus Berges Elzbieta Jankowska Delphine Bard Dave Mark 《Journal of nanoparticle research》2009,11(8):1867-1881
In the past few years, an increasing number of studies on workplace air measurements on manufactured nano-materials and -objects
have been published. Most of the studies had a more explorative character, so a direct interpretation to workers” exposure
for a given exposure situation, activity, or process is not a straight-forward process. In general, the studies use a quite
similar package of devices for near real-time monitoring of particle number- and mass concentration in size ranges <100 nm
up to 10 μm, and the collection of samples for off-line characterization of air samples. Various approaches for addressing
background concentrations and its use to indicate the potential for exposure to nano-objects could be observed. Within the
EU-sponsored NANOSH project, a harmonized approach for measurement strategy, data analysis and reporting was developed. In
addition to time/activity–concentration profiles as reported by most studies, this approach enables a first step to estimate
the potential for exposure to manufactured nano-objects, more quantitatively. The NANOSH data will be collated into a base,
which may form the starting point for a harmonized database facilitating overall analysis in near future, to derive estimates
for exposure for several exposure situations. 相似文献