3585-33-9Relevant articles and documents
Evaluation of Amino Substituants as Nucleofugal Controllers of Regioselectivity and as Chelate Modulators of Stereoselectivity in Squarate Ester Cascades
Paquette, Leo A.,Kuo, Lung Huang,Tae, Jinsung
, p. 2010 - 2021 (1998)
The tandem addition of an alkenyllithium reagent and a 2-lithioallylamine to squarate esters has been systematically examined. The effect of the sequencing of this twofold addition has been investigated. The extent to which the amino group is eliminated was found to be dependent on the structural features of the companion nucleophile. Also assessed was the comparative ease with which the amino and methoxy groups experience competitive β-elimination from the highly reactive, medium-ring dianionic intermediates. Attempts were made to curtail the level of competing 1,4-addition, and success was achieved by increasing the effective size of the O-alkyl groups in the squarate ester. The highly stereocontrolled transformations described represent a notably direct means for producing highly fused polycyclic compounds. Mechanistic considerations surrounding these reactions, which are characterized by an impressive enhancement of molecular scaffolding, are discussed.
Synthesis, Structure, and Reactivity of Ga-Substituted Distibenes and Sb-Analogues of Bicyclo[1.1.0]butane
Tuscher, Lars,Helling, Christoph,Ganesamoorthy, Chelladurai,Krüger, Julia,W?lper, Christoph,Frank, Walter,Nizovtsev, Anton S.,Schulz, Stephan
, p. 12297 - 12304 (2017)
Monovalent gallanediyl LGa {L=HC[C(Me)N(2,6-iPr2C6H3)]2} reacts with SbX3 to form the Ga-substituted distibenes [(LGaX)2Sb2] (X=NMeEt 1, Cl 2). Upon heating, 2 reacts to the bicyclo[1.1.0]butane analogue [(LGaCl)2(μ,η1:1-Sb4)] 3 containing a [Sb4]2? dianion. Moreover, 2 reacts with Li amides LiNR2 in salt elimination reactions that form the corresponding amido-substituted compounds 1 and [(LGaNMe2)2Sb2] 4, whereas reactions of 4 and [(LGaNMe2)2(μ,η1:1-Sb4)] 5 with two equivalents of GaCl3 resulted in the formation of 2 and 3, respectively. 1, 2 and 3 were characterized by 1H and 13C NMR spectroscopy, elemental analysis, and single crystal X-ray diffraction. In addition, their bonding situation was analyzed by quantum chemical calculations.
A nickel(II) guanidinate compound and its potential as CVD precursor for nickel related films
Zhang, Yuxiang,Du, Liyong,Liu, Xinfang,Ding, Yuqiang
, p. 218 - 222 (2018)
In this study, a nickel(II) compound with guanidinate ligand of the general form [((Me)2NC(iPrN)2)2Ni] has been synthesized and isolated from the reaction of NiCl2 with the corresponding lithium salt of guanidinate ligand [(Me)2NC(iPrN)2Li] at 70 °C. Its structure was determined by 1H NMR, elemental analysis, and single crystal X-ray diffraction. Thermogravimetric analysis (TGA) was employed to study the thermal properties (including thermal stability, volatility, vapor pressure and transport behavior) of compound. Furthermore, a deposition experiment was made to examine the compound's potential as CVD precursor, and a Ni metal film was successfully deposited. These preliminary results illustrate the potential of this compound to act as CVD precursor.
Preparation method of beta-caraban
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Paragraph 0057-0060; 0089-0090, (2021/11/10)
The preparation method comprises the following steps: in liquid dimethylamine, a compound of the structural formula II or a salt thereof and MN (CH). 3 )2 The dimethylamine solution in the structural formula I is reacted to obtain the fritilth. M represents Li or MgX; and M is Li or Na. Wherein X is selected from one of Cl, Br and I. The preparation method disclosed by the invention is high in yield and high in product purity, can substantially avoid generation of single methyl ammonia impurities and dechlorination impurities, and greatly simplifies the subsequent refining process. In addition, the preparation method is single in solvent, the use of the mixed solvent is avoided, the later-stage solvent recovery is convenient, and the three wastes can be reduced.
Mesoporous Silica-Supported Amidozirconium-Catalyzed Carbonyl Hydroboration
Eedugurala, Naresh,Wang, Zhuoran,Chaudhary, Umesh,Nelson, Nicholas,Kandel, Kapil,Kobayashi, Takeshi,Slowing, Igor I.,Pruski, Marek,Sadow, Aaron D.
, p. 7399 - 7414 (2015/12/11)
The hydroboration of aldehydes and ketones using a silica-supported zirconium catalyst is reported. Reaction of Zr(NMe2)4 and mesoporous silica nanoparticles (MSN) provides the catalytic material Zr(NMe2)n@MSN. Exhaustive characterization of Zr(NMe2)n@MSN with solid-state (SS)NMR and infrared spectroscopy, as well as through reactivity studies, suggests its surface structure is primarily ≡ SiOZr(NMe2)3. The presence of these nitrogen-containing zirconium sites is supported by 15N NMR spectroscopy, including natural abundance 15N NMR measurements using dynamic nuclear polarization (DNP) SSNMR. The Zr(NMe2)n@MSN material reacts with pinacolborane (HBpin) to provide Me2NBpin and the material ZrH/Bpin@MSN that is composed of interacting surface-bonded zirconium hydride and surface-bonded borane ≡ SiOBpin moieties in an approximately 1:1 ratio, as well as zirconium sites coordinated by dimethylamine. The ZrH/Bpin@MSN is characterized by 1H/2H and 11B SSNMR and infrared spectroscopy and through its reactivity with D2. The zirconium hydride material or the zirconium amide precursor Zr(NMe2)n@MSN catalyzes the selective hydroboration of aldehydes and ketones with HBpin in the presence of functional groups that are often reduced under hydroboration conditions or are sensitive to metal hydrides, including olefins, alkynes, nitro groups, halides, and ethers. Remarkably, this catalytic material may be recycled without loss of activity at least eight times, and air-exposed materials are catalytically active. Thus, these supported zirconium centers are robust catalytic sites for carbonyl reduction and that surface-supported, catalytically reactive zirconium hydride may be generated from zirconium-amide or zirconium alkoxide sites.
HAFNIUM- AND ZIRCONIUM-CONTAINING PRECURSORS AND METHODS OF USING THE SAME
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Page/Page column 13, (2011/02/24)
Disclosed are hafnium- and zirconium-containing precursors and methods of providing the same. The disclosed precursors include a ligand and at least one aliphatic group as substituent selected to have greater degrees of freedom than the usual substituents. The disclosed precursors may be used to deposit hafnium- or zirconium-containing layers using vapor deposition methods such as chemical vapor deposition or atomic layer deposition.
Synthesis and ethylene trimerisation capability of new chromium(II) and chromium(III) heteroscorpionate complexes
Kilpatrick, Alexander F. R.,Kulangara, Shaneesh Vadake,Cushion, Michael G.,Duchateau, Robbert,Mountford, Philip
body text, p. 3653 - 3664 (2010/06/18)
Reaction of (Me2pz)2CHSiMe2N(H)R (R = iPr or Ph) or (Me2pz)2CHSiMe 2NMe2 with CrCl3(THF)3 or CrCl 2(THF)2 gave Cr{(Me2pz)2CHSiMe 2NR1R2}Cl3 (R1 = H, R2 = iPr (10) or Ph (11); R1 = R2 = Me (15)) or Cr{(Me2pz)2CHSiMe2NR 1R2}Cl2(THF) (R1 = H, R2 = iPr (12) or Ph (13); R1 = R2 = Me (16)), respectively. Compounds 10 and 11 were crystallographically characterized and the magnetic behaviour of all the new compounds was evaluated using SQUID magnetometry. Reaction of CrCl3(THF)3 with Li{C(Me 2pz)3}(THF) gave the zwitterionic complex Cr{C(Me 2pz)3}Cl2(THF) (17) containing an apical carbanion. Reaction of the analogous phenol-based ligand (Me2pz) 2CHArOH (ArO = 2-O-3,5-C6H2tBu 2) with CrCl3(THF)3 gave Cr{(Me 2pz)2CHArOH}Cl3 (19) whereas the corresponding reaction with CrCl2(THF)2 unexpectedly gave the Cr(iii) phenolate derivative Cr{(Me2pz)2CHArO}Cl2(THF) (20) which could also be prepared from CrCl3(THF)3 and the sodiated ligand [Na{(Me2pz)2CHArO}(THF)]2. Reaction of the corresponding ether (Me2pz)2CHArOMe with CrCl3(THF)3 or CrCl2(THF)2 gave Cr{(Me2pz)2CHArOMe}Cl3 (23) and Cr{(Me 2pz)2CHArOMe}Cl2(THF) (24), respectively. The catalytic performance in ethylene oligomerisation/polymerisation of all of the new Cr(ii) and Cr(iii) complexes was evaluated. Most of the complexes showed high activity, but produced a Schultz-Flory distribution of α-olefins. Compound 23 had an exceptionally low α-value of 0.37 and showed a preference for 1-hexene and 1-octene formation. While replacing a secondary amine (10-13) for a tertiary amine (15-16) resulted in loss of catalytic activity, replacing a phenol (19) for an anisole (23) group afforded a more selective and more active catalyst. Changing from MAO to DIBAL-O as cocatalyst induced a switch in selectivity to ethylene polymerisation.
METHODS OF SYNTHESIZING PHARMACEUTICAL SALTS OF A FACTOR XA INHIBITOR
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Page/Page column 42-43, (2008/12/05)
Novel methods of preparing a compound of Formula I which is an inhibitor of Factor Xa and its maleate salt, are described herein.
Novel pharmaceutical salts and polymorphs of a factor Xa inhibitor
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Page/Page column 9, (2008/06/13)
The present invention provides for salts comprising a compound of Formula I and an acid that has activity against mammalian factor Xa. The present invention is also directed to methods of making the compound of Formula I.
Organometallic compound, its synthesis method, and solution raw material and metal-containing thin film containing the same
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Page 6, (2008/06/13)
The organometallic compound of the present invention is a compound that has bonds between metal atoms and nitrogen atoms or bonds between semimetal atoms and nitrogen atoms, and the content of chlorine in the compound is 200 ppm or less and the content of water is 30 ppm or less. In addition, the general formula of this compound is represented by the following formula (1): M[(R1)2N](n?s)(R2)s??(1) wherein, M represents a metal atom or semimetal atom, with the metal atom being Hf, Zr, Ta, Ti, Ce, Al, V, La, Nb or Ni, and the semimetal atom being Si, R1 represents a methyl group or ethyl group, R2 represents an ethyl group, n represents the valence of M, and s represents an integer of 0 to n?1.
