- Method for preparing kakonein derivatives
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The invention discloses a puerarin derivative preparation method. Puerarin derivative has the structural formula as shown in the specification, and the puerarin derivative is obtained by that puerarin reacts with CH2(R)2, wherein R is a tertiary amine gene. The puerarin derivative preparation method is characterized in that reaction is carried out under hydrochloric acid catalysis. Compared with the prior art, the puerarin derivative preparation method is characterized in that the yield of a puerarin derivative product can be obviously improved after the class of reaction adopts hydrochloric acid catalysis.
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Paragraph 0025-0026
(2017/03/17)
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- Siloxymethylamines as Aminomethylation Reagents for Amines Leading to Labile Diaminomethanes That can be Trapped as Their [Mo(CO)4] Complexes
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Compound Et3SiOCH2NMe2 transfers Me2NCH2 to R2NH (R2=Et2, PhMe, [Cr(η6-C6H5)(CO)3]Me, PhH) to form previously unknown diaminomethanes, Me2NCH2NR2 and, in the case of R2=PhH, the triamine Me2NCH2N(Ph)CH2NMe2. The diaminomethanes exhibit an unreported disproportionation to a mixture of (R2N)2CH2, (Me2N)2CH2, and Me2NCH2NR2, which can be trapped as their [Mo(CO)4(diamine)] complexes. Whereas PhMeNCH2NMe2 is a labile material, the metal-substituted ([(η6-C6H5)Cr(CO)3]MeNCH2NMe2 is a stable material. The triamine Me2NCH2N(Ph)CH2NMe2 is unstable with respect to transformation to 1,3,5-triphenyltriazine, but is readily trapped as the bidentate-triamineMo(CO)4. All metal complexes were characterized by single-crystal X-ray diffraction.
- Sharma, Hemant K.,Gonzalez, Paulina E.,Craig, Alexander L.,Chakrabarty, Sanchita,Metta-Maga?a, Alejandro,Pannell, Keith H.
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p. 7363 - 7366
(2016/05/24)
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- Preparation of all N-coordinated zirconium amide amidinates and studies of their reactions with dioxygen and water
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Zr(NR2)2[MeC(NiPr)2]2 (R = Me, 1; Et, 2) have been prepared through aminolysis and their reactions with O2 and water have been studied. Two major products from the reactions are the oxo dimer {(μ-O)Zr[MeC(NiPr)2]2}2 (3) and its insoluble polymer {(μ-O)Zr[MeC(NiPr)2]2}n (4). Over time the dimer 3 polymerizes to 4. Zr peroxo trimer {(μ-η2:η2-O2)Zr[MeC(NiPr)2]2}3 (5) was also observed from the reaction of 1 with O2 and its crystal structure is reported. DFT calculations show that the reaction of 1 with O2 follows a radical process, yielding the peroxo trimer 5. Mass spectrometric studies of the reactions of water in air with 1 and 2 show the formation of the oxo monomer (O=)Zr[MeC(NiPr)2]2 (6), oxo dimer {(μ-O)Zr[MeC(NiPr)2]2}2 (3), and the dihydroxy monomer (HO)2Zr[MeC(NiPr)2]2 (7). In addition, the cations {Zr(NR2)[MeC(NiPr)2]2}+ (R = Me, Et) were observed. 2 revealed an interesting dynamic NMR behavior. Variableerature (VT) NMR spectroscopy has been used to study the Bailar twist process in 2, giving activation parameters ΔH? = 10.9(1.1) kcal mol-1, ΔS? = -11(4) eu and ΔG?303 K = 14(2) kcal mol-1.
- Lamb, Adam C.,Wang, Zheng,Cook, Tabitha M.,Sharma, Bhavna,Chen, Shu-Jian,Lu, Zheng,Steren, Carlos A.,Lin, Zhenyang,Xue, Zi-Ling
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- Reactions of zirconium amide amidinates with dioxygen. Observation of an unusual peroxo intermediate in the formation of oxo compounds
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Reaction of d0 Zr(NMe2)2[MeC(N iPr)2]2 (1) with O2 at -30°C gives three Zr containing products: a peroxo trimer {(μ-η2: η2-O2)Zr[MeC(NiPr)2] 2}3 (2), an oxo dimer {(μ-O)Zr[MeC(N iPr)2]2}2 (3), and an oxo polymer {(μ-O)Zr[MeC(NiPr)2]2}n (4). 2 is a rarely observed peroxo complex from the reaction of a d0 complex with O2. This journal is the Partner Organisations 2014.
- Lamb, Adam C.,Lu, Zheng,Xue, Zi-Ling
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supporting information
p. 10517 - 10520
(2014/12/10)
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- Reactions of group 4 amide guanidinates with dioxygen or water. Studies of the formation of oxo products
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Reactions of the zirconium amide guanidinates (R2N) 2M[iPrNC(NR2)NiPr]2 (R = Me, M = Zr, 1; M = Hf, 2; R = Et, M = Zr, 3) with O2 or H 2O give products that are consistent with the oxo dimers {M(μ-O)[iPrNC(NR2)NiPr]2} 2 (R = Me, M = Zr, 4; M = Hf, 5; R = Et, M = Zr, 6) and polymers {M(μ-O)[iPrNC(NR2)NiPr]2} n (R = Me, M = Zr, 7; M = Hf, 8; R = Et, M = Zr, 9). Mass spectrometric (MS) analyses of the reactions of water in air with 1 and 2 show formation of the Zr monomer Zr(=O)[iPrNC(NMe2)N iPr]2 (10), oxo dimers 4 and 5, and dihydroxyl complexes M(OH)2[iPrNC(NMe2)NiPr]2 (M = Zr, 11; Hf, 12). Similar MS analyses of the reaction of diethylamide guanidinate 3 with water in air show the formation of Zr(=O)[ iPrNC(NEt2)NiPr]2 (13), Zr(OH) 2[iPrNC(NEt2)NiPr]2 (14), 6, and {(Et2N)Zr[iPrNC(NEt2)N iPr]2}+ (15). Kinetic studies of the reaction between 1 and a continuous flow of 1.0 atm of O2 at 80-105 C indicate that it follows pseudo-first-order kinetics with ΔH? = 8.7(1.1) kcal/mol, ΔS? = -54(3) eu, ΔG ?358 K = 28(2) kcal/mol, and a half-life of 213(1) min at 85 C.
- Sharma, Bhavna,Callaway, Tabitha M.,Lamb, Adam C.,Steren, Carlos A.,Chen, Shu-Jian,Xue, Zi-Ling
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supporting information
p. 11409 - 11421
(2013/10/22)
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- Synthesis and aminomethylation of 7-hydroxy-5-methoxyisoflavones
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A synthetic method for 7-hydroxy-5-methoxyisoflavones starting from 5,7-dihydroxyisoflavones was developed. Dimethylcarbamoylchloride was proposed for protection of the 7-hydroxy group. Aminomethylation of the synthesized 7-hydroxy-5-methoxyisoflavones by formaldehyde aminals was studied.
- Mrug,Bondarenko,Khilya,Frasinyuk
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p. 235 - 241
(2013/07/26)
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- Photophysical properties and OLED performance of light-emitting platinum(ii) complexes
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The synthesis, photophysical properties and application as emitters in solution-processed multi-layer organic light-emitting diodes (OLEDs) of a series of blue-green to red light-emitting phosphorescent platinum(ii) complexes are reported. These complexes consist of phenylisoquinoline, substituted phenylpyridines or tetrahydroquinolines as C^N cyclometalating ligands and dipivaloylmethane as an ancillary ligand. Depending on both the structure of the C^N cyclometalating ligands and the dopant concentration in the matrix, these platinum(ii) complexes exhibit different aggregation tendencies. This property affects the photoluminescence spectra of the investigated compounds and colour-stability of the fabricated OLEDs. Using the blue-green to yellow-green emitting complexes, the best results were obtained with the 2-(4- trifluoromethylphenyl)-5,6,7,8-tetrahydroquinoline based platinum(ii) complex. A maximum luminous efficiency of 4.88 cd A-1 and a power efficiency of 4.65 lm W-1, respectively, were achieved. Employing the red emitting phenylisoquinoline based complex as an emitter, colour-stable and efficient (4.71 cd A-1, 5.12 lm W-1) devices were obtained.
- Kourkoulos, Dimitrios,Karakus, Cüneyt,Hertel, Dirk,Alle, Ronald,Schmeding, Sebastian,Hummel, Johanna,Risch, Nikolaus,Holder, Elisabeth,Meerholz, Klaus
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supporting information
p. 13612 - 13621
(2013/09/23)
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- Oxygen and temperature sensitivity of blue to green to yellow light-emitting Pt(ii) complexes
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The synthesis and photophysical properties of a series of yellow-green to blue-green emitting heteroleptic, cyclometalated Pt(ii)(acac) complexes based on substituted phenylpyridine and tetrahydroquinoline ligands is reported. The luminescence intensities and lifetimes of these compounds were also studied in poly(styrene) films with respect to their responses to oxygen and temperature. Particularly, due to the insensitivity to oxygen quenching, these complexes are promising candidates as inert reference dyes in optical sensors. On the other hand, the Pt(ii) complex with 2-(4-bromophenyl)-5,6,7,8-tetrahydroquinoline as C^N ligand, displays a strong temperature quenching effect. The distinct response to temperature was additionally calibrated after incorporation in poly(vinylidene chloride-co-acrylonitrile) serving as oxygen-blocking matrix copolymer. The resulting yellow-green-emitting temperature sensor signifies an interesting alternative to the available mostly red emitting temperature-sensitive probes.
- Karakus, Cueneyt,Fischer, Lorenz H.,Schmeding, Sebastian,Hummel, Johanna,Risch, Nikolaus,Schaeferling, Michael,Holder, Elisabeth
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experimental part
p. 9623 - 9632
(2012/08/28)
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- Substituted Sulfonamide Compounds
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Substituted sulfonamide compounds corresponding to the formula I wherein m, n, p, Q, R1, R2, R3, R4, X, Y and Z have the respective meanings defined herein, pharmaceutical compositions containing such compounds, a process for their preparation, and the use of such compounds for the treatment and/or inhibition of pain and other conditions mediated by bradykinin receptor 1 (B1R) and/or bradykinin receptor 2 (B2R).
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Page/Page column 36
(2009/07/25)
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- SUBSTITUTED SULFONAMIDE DERIVATIVES
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The invention relates to substituted sulfonamide derivatives of the general formula (I'); processes for their preparation, medicaments containing these compounds, and the use of substituted sulfonamide derivatives for the preparation of medicaments
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Page/Page column 109
(2009/08/16)
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- α-dicarbonylmonoximes as nucleophiles and neighbour groups
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The α-dicarbonylmonooximes 1 and 11 do not react as simple "CH-acidic-compounds" in the Mannich condensation. In a concerted reaction with aminals in absolute dioxane they give rise to the products 4a - e and 12a - e with better practicability and much higher yields compared with the conventional method. The Mannich bases with a cyclic amine part show in the dehydrogenation, using mercury-EDTA, a neighbouring group participation of the oxime in type 4 and of the oxime or amide function in 12 yielding cyclized products. For the reaction a plausible mechanism is proposed.
- M?hrle, Hans,Keller, Georg
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p. 632 - 642
(2007/10/03)
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- Thermal decomposition of 2,6-di-tert-butyl-4-dimethylaminomethylphenol
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Products of thermolysis of 2,6-di-tert-butyl-4-dimethylaminomethylphenol were determined qualitatively and quantitatively by GLC, UV, and 1H NMR methods. The kinetics of the reaction was studied. The thermolysis products were studied as the inhibitors in thermopolymerization of monomers.
- Zakharova,Khismatullina,Ivanov
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p. 1787 - 1789
(2007/10/03)
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- The generation of iminium ions using chlorosilanes and their reactions with electron rich aromatic heterocycles
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Dichlorodimethylsilane and trichloromethylsilane have been used to generate iminium ions from aminals and aminol ethers derived from secondary alkylamines, including glycine derivatives, in aprotic media which were shown to undergo reactions with electron rich aromatic heterocycles, including furan, to give mono-aminoalkylation products in good yields. Whereas chlorotrimethylsilane has been shown to generate iminium ions from aminol ethers, no evidence was adduced for the involvement of iminium ions using aminals. 2,5-Disubstitution of N-methylpyrrole was the major result in reactions of N-methylpyrrole with aminals in the presence of chlorotrimethylsilane where no build up of hydrogen chloride occurs and where chlorotrimethylsilane can function catalytically. Experimental results, including the use of bis(trimethylsilyl)acetamide as a proton scavenger, and some relative rate data, are presented that allow possible mechanisms to be evaluated.
- Heaney, Harry,Papageorgiou, George,Wilkins, Robert F.
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p. 2941 - 2958
(2007/10/03)
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- Titanium Catalyzed Reduction of Aromatic Halides by Sodium Borohydride
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The reduction of aryl halides by sodium borohydride is catalyzed by titanium complexes; di(cyclopentadienyl)titanium dichloride (titanocence dichloride) is highly effective.The reaction scope and mechanism are solvent dependent.In dimethylformamide (DMF), an adduct of DMF and sodium borohydride is formed which reduces simple aryl halides by a non-radical, likely nucleophilic route.Dimethylamino- substituted products are formed, as are simple dechlorinated species.In dimethylacetamide or in ethers, a radical-based reaction involving activated titanocene borohydride takes place, and only dechlorinated products result.
- Liu, Yumin,Schwartz, Jeffrey
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p. 4471 - 4482
(2007/10/02)
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- 3,4-N,trisubstituted-4,5-dihydro-1H-pyrazole-1-carboxamides and their use as insecticides
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3,4,N-Trisubstituted-4,5-dihydro-1H-pyrazole-1-carboxamide compounds wherein the substituent in the 4-position is a 5-membered heterocyclic ring moiety containing one ring oxygen or sulfur atom and one or two ring nitrogen atoms and the substituents in the 3-position and the N-position are optionally substituted phenyl moieties, such as 4,5-dihydro-3-(4-fluorophenyl)-N-(4-trifluoromethylphenyl)-4-(2-trifluoromethyl-5-thiazolyl)-1H-pyrazole-1-carboxamide were prepared from appropriate 3,4-disubstituted-4,5-dihydro-1H-pyrazole compounds, such as 4,5-dihydro-3-(4-fluorophenyl)-4-(2-trifluoromethyl-5-thiazolyl)-1H-pyrazole and phenyl isocyanates and isothiocyanates, such as 4-(trifluoromethyl)phenyl isocyanate. The compounds are insecticidal.
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- Process for converting heat stable amine salts to heat regenerable amine salts
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Processes are disclosed for converting heat stable amine salts to heat regenerable amine salts using a modified electrodialysis zone (140). The processes of the present invention can be used to reduce the level of heat stable salts in a lean solvent stream in an acid gas removal process and can be integrated with the acid gas removal process to utilize process streams as a source of ions.
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- Preparation of silane and amine alanes
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Process for the preparation of silane and a tertiary amine alane, said process comprising reacting: (a) an alkali metal aluminum tetrahydride having the formula MAlH4, wherein M is an alkali metal selected from the class consisting of lithium, sodium and potassium, (b) silicon tetrachloride, and (c) a complexing tertiary amine, such that the molar proportion of (a) to (b) to (c) is about 4:1:4. In this process, NaAlH4 and triethylamine are preferred reactants. The amine alane product can be reacted with additional silicon halide to prepare additional silane. This step can be conducted utilizing amine alane in the reaction mixture produced by the process above, and is preferably conducted using SiF4 as the silicon tetrahalide to produce AlF3 as a co-product. Both AlF3 and silane are valuable articles of commerce.
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- Preparation of amine alanes
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Process for the preparation of an amine alane, said process comprising reacting: (a) an alkali metal aluminum tetrahydride having the formula MAlH4, wherein M is an alkali metal selected from the class consisting of lithium, sodium and potassium, (b) a hydrogen halide, and (c) a complexing tertiary amine. In this process, NaAlH4, HCl, and (C2H5)3N are preferred reactants.
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- AMINE RADICAL CATIONS : AN ELECTRON SPIN RESONANCE STUDY OF CATIONS GENERATED BY RADIOLYSIS
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Amine radical cations have been generated by exposing dilute solutions of amines to 60Co γ-rays at 77 K.They are well characterised by their e.s.r. spectra, the method and interpretation being established by showing that the e.s.r. data for Me3N(.+) cations are indentical with literature values.Results for the triethylammonium cation show that the β-protons do not occupy the most favourable sites for maximum hyperconjugation, in contrast with other radical cations.This is explained in terms of steric factors, and an equilibrium between two preferred conformations. 1,1-Diamines, R2NCH2NR2, give cations having localised structures, R2N(.+)CH2NR2, rather than the delocalised structure adopted by acetal cations.Possible evidence for weak N-N bonding and delocalisation is adduced for NN'-dimethylpiperazine cations, but we confirm that the cation of triethylenediamine has a truly delocalised ?(*) structure.There is no tendency for R3N(+.) cations to react with neutral amines to give ( dimer cations, in marked constrast with results for corresponding trialkylphosphine systems.
- Eastland, George W.,Rao, D. N. Ramakrishna,Symons, Martyn C. R.
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p. 1551 - 1558
(2007/10/02)
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