544-97-8Relevant academic research and scientific papers
Nucleation and growth of ZnO in organic solvents - An in situ study
Lizandara-Pueyo,Van Den Berg,De Toni,Goes,Polarz
, p. 16601 - 16610 (2008)
ZnO is a metal oxide material which possesses versatile properties and applications. Therefore, the target-oriented preparation of ZnO has become a major issue. Many preparation techniques involve bottom-up methods from precursor solutions. In the current contribution, a special precursor system is described that enables a fine-control of kinetic parameters for the nucleation and growth of ZnO in various organic solvents. A large variety of analytical techniques could be applied in an in situ fashion to probe for the ZnO formation at all times and all length scales. Among the analytical techniques are UV/vis, Raman, Fluorescence, X-ray absorption, 1H NMR-spectroscopy, dynamic light-scattering, and TEM. Three different regimes for nucleation and growth with different characteristics could be identified. Furthermore, the effect of different parameters on the resulting ZnO particle size was investigated.
Selective oxidation of the alkyl ligand in rhenium(V) oxo complexes
DuMez, Darin D.,Mayer, James M.
, p. 12416 - 12423 (1996)
Rhenium(V) oxo alkyl triflate compounds (HBpz3)ReO(R)OTf [R = Me (4), Et (5), n-Bu (6); HBpz3 = hydrotris(1-pyrazolyl)borate; OTf = OSO2CF3, triflate] are formed on sequential reaction of (HBpz3)ReOCl2 with dialkyl zinc reagents and AgOTf. These triflate compounds are rapidly oxidized at ambient temperatures by oxygen atom donors pyridine N-oxide (pyO) and dimethyl sulfoxide (DMSO) to give (HBpz3)ReO3 (7) and the corresponding aldehyde. In the cases of 5 and 6 this transformation is quantitative. The addition of 2,6-lutidine to a low-temperature oxidation of 5 by DMSO redirects the reaction to form cis-2-butene instead of acetaldehyde. These oxidation reactions do not proceed through alkoxide intermediates, as shown by independent studies of alkoxide oxidations. Reaction of 5 with pyO or DMSO at -47°C results in the formation of intermediates which are assigned as ylide or 'trapped-carbene' complexes [(HBpz3)ReO(OH){CH(L)CH3}]OTf (L = py (8) or SMe2 (9), respectively). Mechanistic studies and analogies with related systems suggest that oxygen atom transfer to 4-6 forms [(HBpz3)ReO2R]+. Transfer of an α-hydrogen from the alkyl group to an oxo ligand then forms an alkylidene complex which is trapped by SMe2 or py to give the observed intermediates. Further oxidation of the ylide complex gives the aldehyde.
Electrophilic Amination with Nitroarenes
Rauser, Marian,Ascheberg, Christoph,Niggemann, Meike
supporting information, p. 11570 - 11574 (2017/09/11)
An exceptionally general electrophilic amination, which directly transforms commercially available nitroarenes into alkylated aromatic aminoboranes with zinc organyl compounds was developed. The reaction starts with a two-step partial reduction of the nitro group to a nitrenoid, which is used in situ as the electrophilic amination reagent. To facilitate isolation, the resulting air- and moisture-sensitive aminoboranes were reacted with a range of electrophiles. The method not only represents a direct transformation of nitro compounds into electrophilic amination reagents but also provides an elegant alternative to dehydrocoupling methods for the generation of aminoboranes.
A dimethyl zinc preparation method
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Paragraph 0017-0019, (2020/02/10)
The invention belongs to a preparation method for dimethylzinc. The method includes the following steps that zinc halide is added into a reaction kettle under inert gas protection, then trimethylaluminum is dropwise added under the stirring condition, the reaction speed is controlled through the addition speed of the trimethylaluminum, stirring continues for reaction of 3 h-5 h after addition of the trimethylaluminum is finished, then the temperature of the reaction kettle is adjusted to be 42 DEG C-90 DEG C and kept for 2 h-3 h, and distilled Zn(CH3)2 is collected; diethylzinc is dropwise added into the reaction kettle, the temperature of the reaction kettle is controlled to be 91 DEG C-120 DEG C, distilled Zn(CH3)2 is collected, the temperature of the reaction kettle is kept within 91 DEG C-120 DEG C after addition of the diethylzinc is finished, and Zn(CH3)2 continues being collected for 1 h-3 h. According to the method, raw materials of the dimethylzinc are easy to get, reaction is simple, control is easy, industrial production is facilitated, the reaction yield is high, and the total yield reaches more than 90%.
Molecular Zinc Species with Ge-Zn and Sn-Zn Bonds: A Reversible Insertion of a Stannylene into a Zinc-Carbon Bond
Erickson, Jeremy D.,Riparetti, Ryan D.,Fettinger, James C.,Power, Philip P.
supporting information, p. 2124 - 2128 (2016/07/11)
The tetrylenes Ge(ArMe6)2 and Sn(ArMe6)2 (ArMe6 = C6H3-2,6-(C6H2-2,4,6-(CH3)3)2) reacted with dimethylzinc to afford the insertion products (ArMe6)2Ge(Me)ZnMe (1) and (ArMe6)2Sn(Me)ZnMe (3), which feature Ge-Zn and Sn-Zn bonds as well as two-coordinate zinc atoms. Crystals of 1 were found to be unsuitable for X-ray crystallography, so the ethyl-substituted (ArMe6)2Ge(Et)ZnEt (2) was synthesized in a parallel way to provide crystals suitable for X-ray studies. These showed the structure to be similar to that of 3. The reaction of Pb(ArMe6)2 with dimethylzinc yielded ArMe6ZnMe with a linearly coordinated zinc atom via ligand exchange but no characterizable, new lead product was obtained. The reaction of Sn(ArMe6)2 with dimethylzinc is reversible in hydrocarbon solution at room temperature and displayed a dissociation constant Kdiss and a ΔGdiss of 0.0028(5) and 14(4) kJ mol-1 at 298 K, respectively. Compounds 1-4 were characterized by NMR and IR spectroscopy as well as by X-ray crystallography for 1, 3, and 4.
Exchange of alkyl and tris(2-mercapto-1-t-butylimidazolyl)hydroborato ligands between zinc, cadmium and mercury
Kreider-Mueller, Ava,Quinlivan, Patrick J.,Rong, Yi,Owen, Jonathan S.,Parkin, Gerard
, p. 177 - 183 (2015/08/18)
Abstract The tris(2-mercaptoimidazolyl)hydroborato ligand, [TmBut], has been used to investigate the exchange of alkyl and sulfur donor ligands between the Group 12 metals, Zn, Cd and Hg. For example, [TmBut]2Zn reacts with Me2Zn to yield [TmBut]ZnMe, while [TmBut]CdMe is obtained readily upon reaction of [TmBut]2Cd with Me2Cd. Ligand exchange is also observed between different metal centers. For example, [TmBut]CdMe reacts with Me2Zn to afford [TmBut]ZnMe and Me2Cd. Likewise, [TmBut]HgMe reacts with Me2Zn to afford [TmBut]ZnMe and Me2Hg. However, whereas the [TmBut] ligand transfers from mercury to zinc in the methyl system, [TmBut]HgMe/Me2Zn, transfer of the [TmBut] ligand from zinc to mercury is observed upon treatment of [TmBut]2Zn with HgI2 to afford [TmBut]HgI and [TmBut]ZnI. These observations demonstrate that the phenomenological preference for the [TmBut] ligand to bind one metal rather than another is strongly influenced by the nature of the co-ligands.
Nickel-catalyzed C-F bond activation and alkylation of polyfluoroaryl imines
Yang, Xiuxiu,Sun, Hongjian,Zhang, Shumiao,Li, Xiaoyan
, p. 36 - 42 (2013/02/21)
In this paper we show the C-F bond activation and alkylation in polyfluoroaryl imines. An active trimethylphosphine supported nickel-catalyzed cross-coupling reaction of polyfluoroaryl imines with ZnMe2 under mild conditions is described. According to the in situ 19F NMR spectroscopic data, the substrates are quantitatively converted into di-methylation products, while mono-methylation can also be realized under the controlled conditions in moderate yields. Apart from ZnMe2, other organozinc regents were tried in this system. However, due to the nucleophilicity and steric hindrance, they show much lower reactivity than ZnMe2. Only in the case of benzylic zinc chloride, the dibenzylation product can be obtained quantitatively by raising temperature to 90 °C. The results reported here will benefit the development of C-F bond activation as well as the diversity of Schiff bases.
Fused Bicyclic Kinase Inhibitors
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Page/Page column 23-24, (2011/11/30)
Compounds of Formula I, as shown below and defined herein: pharmaceutically acceptable salts thereof, synthesis, intermediates, formulations, and methods of disease treatment therewith, including treatment of cancers, such as tumors driven at least in part by at least one of RON, MET or ALK. This Abstract is not limiting of the invention.
METHODS FOR PREPARING DIORGANOZINC COMPOUNDS
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Page/Page column 20, (2009/01/20)
There are provided methods for preparing the diorganozmc compounds of formula R2Zn (I or Ia), where R is a defined organic radical, and the two R groups can be the same or different The starting material is the zinc compound ZnX2 (II) or R2ZnX (IIa), where X is a defined anion and R2 is a defined organic radical. The zinc reagent of type II is combined with a Grignard reagent and also, when X is Cl or Br, with an alkali metal reagent (VI) to form the diorganozinc product (I or Ia). Also provided are methods for preparing the zinc alcoholates of formula Zn(OR1)2 by reaction of ZnX2, where X = Cl or Br, with an alkali metal reagent of the formula MOR1, where M = Na or K, and where R1 is a defined organic radical.
CRF1 RECEPTOR LIGANDS COMPRISING FUSED BICYCLIC HETEROARYL MOIETIES
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Page/Page column 85, (2008/12/07)
Substituted heteroaryl fused pyridine, pyrazine, and related heterobicyclic compounds that act as selective modulators of CRF1 receptors are provided. These compounds are useful in the treatment of a number of CNS and periphereal disorders, particularly stress, anxiety, depression, cardiovascular disorders, gastrointestinal disorders, and eating disorders. Methods of treatment of such disorders as well as packaged pharmaceutical compositions are also provided. Compounds provided herein are also useful as probes for the localization of CRF receptors and as standards in assays for CRF receptor binding. Methods of using the compounds in receptor localization studies are given.
