- Nitric oxide reduction of copper(II) complex with tetradentate amine ligand followed by ligand transformation
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Copper(II) complex 1 with a tetradentate ligand L [L = tris(2-aminoethyl)amine, tren] has been prepared as its perchlorate salt. Single crystal X-ray structure of 1 indicates its trigonal bipyramidal shape in the solid state. The complex, in dry and degassed acetonitrile solvent, was made to react with nitric oxide gas and the copper(II) center has been observed to reduce to Cu(I) with simultaneous nitrosation followed by diazotization at the terminal primary amine positions of the ligand to result into cyclization product, 1-(2-aminoethyl)piperzine, L′ along with tris(2-aminoethyl)ammonium perchlorate, L′′-perchlorate. However, when an acetonitrile:water (10:1, v/v) mixture has been used as the solvent, the reduction of Cu(II) to Cu(I) is observed and the ligand is found to be precipitated out only as L′′-perchlorate. The reduction of Cu(II) to Cu(I) has been studied by UV-visible, 1H NMR and EPR spectroscopic techniques and by X-ray single crystal structure determination. Both the L′ and L′′-perchlorate have been isolated from the reaction mixture and characterized by using microanalytical studies, various spectroscopic techniques and X-ray single crystal structure determination.
- Sarma, Moushumi,Singh, Amardeep,Gupta G., Subrahmanyam,Das, Gopal,Mondal, Biplab
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- MANUFACTURING METHOD OF CYCLIC ETHYLENE AMINES
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PROBLEM TO BE SOLVED: To provide a method for manufacturing cyclic ethylene amines at good selectivity. SOLUTION: By using a solid catalyst containing palladium or palladium and gold with percentage of palladium of 50 to 100 mol%, ethylene diamine is deamination condensed. SELECTED DRAWING: None COPYRIGHT: (C)2017,JPOandINPIT
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Paragraph 0037; 0040
(2017/08/15)
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- BLENDS OF AMINES WITH PIPERAZINE FOR CO2 CAPTURE
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Compositions and methods related to the removal of acidic gas. In particular, the present disclosure relates to a composition and method for the removal of acidic gas from a gas mixture using a solvent comprising a blend of piperazine and at least one diamine or triamine.
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Page/Page column
(2015/03/16)
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- Amination process for manufacturing amines using catalyst
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Disclosed is a process for the preparation of an amine (particularly diamines and polyamines) by reacting an alkanolamine or a polyol with ammonia in the presence of a catalyst composed of two active metals from the group of transition metals, namely nickel and chromium supported on a microporous refractory substrate, in a hydrogenated, trickle bed reactor.
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Paragraph 0044-0049
(2014/08/07)
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- Unknown
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A process for preparing amines of the formula (II) [in-line-formulae]R1—NH—CH2—CH2—NH2??(II)[/in-line-formulae]in which R1 is hydrogen or radicals of the formula x is integers from zero to two, by reacting nitriles of the formula (I) [in-line-formulae]R2—NH—CH2—CN??(I)[/in-line-formulae]in which R2 is hydrogen or radicals of the formula and R3 is the NC— or H2N—CH2- radicals and x is integers from zero to two, with hydrogen in the presence of a catalyst in suspension mode or in a fixed bed, wherein the space velocity on the catalyst, based on the catalyst surface area, is 10?6 to 10?4 kg of nitrile of the formula (I) per m2 of catalyst surface area and hour, the catalyst surface area being determined by the BET method.
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Paragraph 0588; 0589; 0590; 0591
(2013/04/13)
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- PROCESS FOR PREPARING EDDN AND/OR EDMN AND A PROCESS FOR PREPARING DETA AND/OR TETA
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A process for preparing EDDN and/or EDMN by a) conversion of FA, HCN and EDA, the conversion being effected in the presence of water,b) depleting water from the reaction mixture obtained in stage a), andc) treating the mixture from stage b) with an absorbent in the presence of an organic solvent, wherein the adsorbent is a solid acidic adsorbent.
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Paragraph 0559; 0560; 0562; 0563; 0564; 0565; 0566
(2013/03/26)
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- PROCESS FOR PREPARING EDDN AND EDMN
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A process for preparing EDDN and/or EDMN by conversion of FA, HCN and EDA, the reaction being effected in the presence of water, and, after the conversion, water being depleted from the reaction mixture in a distillation column, which comprises performing the distillation in the presence of an organic solvent which has a boiling point between water and EDDN and/or EDMN at the distillation pressure existing in the column or which forms a low-boiling azeotrope with water.
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Paragraph 0572; 0573; 0578; 0579; 0580
(2013/04/10)
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- Process for Preparing Piperazine
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Process for preparing piperazine of the formula I by reacting diethanolamine (DEOA) of the formula II with ammonia in the presence of hydrogen and a supported, metal-containing catalyst has been found, wherein the catalytically active mass of the catalyst, prior to its reduction with hydrogen, comprises oxygen-containing compounds of aluminum, copper, nickel and cobalt and in the range from 0.2 to 5.0% by weight of oxygen-containing compounds of tin, calculated as SnO, and the reaction is carried out in the liquid phase at an absolute pressure in the range from 160 to 220 bar, a temperature in the range from 180 to 220° C., using ammonia in a molar ratio to DEOA used of from 5 to 25 and in the presence of 0.2 to 9.0% by weight of hydrogen, based on the total amount of DEOA used and ammonia.
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Paragraph 0106; 0107
(2014/01/08)
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- Process for Preparing Piperazine
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Process for preparing piperazine of the formula I by reacting diethanolamine (DEOA) of the formula II with ammonia (NH3) in the presence of hydrogen and a supported, metal-containing catalyst, wherein the catalytically active mass of the catalyst, prior to its reduction with hydrogen, comprises 20 to 85% by weight of oxygen-containing compounds of zirconium, calculated as ZrO2, 1 to 30% by weight of oxygen-containing compounds of copper, calculated as CuO, 14 to 70% by weight of oxygen-containing compounds of nickel, calculated as NiO, and 0 to 5% by weight of oxygen-containing compounds of molybdenum, calculated as MoO3, and the reaction is carried out in the liquid phase at an absolute pressure in the range from 160 to 220 bar, a temperature in the range from 180 to 220° C., using ammonia in a molar ratio to DEOA used of from 5 to 20 and in the presence of 0.2 to 9.0% by weight of hydrogen, based on the total amount of DEOA used and ammonia.
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Paragraph 0097; 0098
(2014/01/08)
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- Process for preparing TETA and DETA
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A process for preparing TETA and/or DETA by hydrogenating EDDN and/or EDMN with hydrogen in the presence of a catalyst, which comprises preparing EDDN and/or EDMN from FA, HCN and EDA in the presence of toluene as a solvent and performing the hydrogenation in suspension mode in the presence of THF.
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Paragraph 0589-0598
(2013/04/13)
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- Dendritic polymers with enhanced amplification and interior functionality
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Poly(ester-acrylate) and poly(ester/epoxide) dendrimers. These materials can be synthesized by utilizing the so-called “sterically induced stoichiometric” principles. The preparation of the dendrimers is carried out by reacting precursor amino/polyamino-functional core materials with various branch cell reagents. The branch cell reagents are dimensionally large, relative to the amino/polyamino-initiator core and when reacted, produce generation=1 dendrimers directly in one step. There is also a method by which the dendrimers can be stabilized and that method is the reaction of the dendrimers with surface reactive molecules to pacify the reactive groups on the dendrimers.
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- NOVEL METHOD FOR PRODUCING TETA BY MEANS OF EDDN
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The invention relates to a process for preparing triethylenetetramine (TETA), which, comprises the following steps: a) reaction of ethylenediamine (EDA) with formaldehyde and hydrocyanic acid (HCN) in a molar ratio of EDA to formaldehyde to HCN of from 1:1.5:1.5 to 1:2:2 to give ethylenediaminediacetonitrile (EDDN),b) hydrogenation of the EDDN obtained in step a) in the presence of a catalyst and a solvent.
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Page/Page column 8-9; 11
(2010/06/11)
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- METHOD FOR PRODUCING TRIETHYLENETETRAMINE
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The invention relates to a process for preparing triethylenetetramine (TETA), which comprises hydrogenating ethylenediaminediacetonitrile (EDDN) in the presence of a catalyst and a solvent.
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Page/Page column 8
(2010/03/02)
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- METHOD FOR PRODUCING TETRAETHYLENEPENTAMINE
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The invention relates to a process for preparing tetraethylenepentamine (TEPA) by hydrogenation of diethylenetriaminediacetonitrile (DETDN) over a catalyst. If appropriate, DETDN can also be present as a constituent of an amino nitrile mixture which additionally comprises diethylenetriaminemonoacetonitrile (DETMN).
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Page/Page column 8
(2010/03/02)
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- PRODUCTION METHOD FOR ETHYLENEAMINE MIXTURES
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The invention relates to a process for preparing an ethylene amine mixture, which comprises hydrogenating an amino nitrile mixture comprising at least two α-amino nitriles in an amount of at least 5% by weight in each case in the presence of a catalyst and, if appropriate, a solvent.
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Page/Page column 10
(2010/05/13)
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- METHODS OF MAKING CYCLIC, N-AMINO FUNCTIONAL TRIAMINES
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The present invention provides strategies for making cyclic triamines. Reactant media including certain precursors and/or certain types of catalysts can be converted into cyclic triamines with improved conversion and selectivity. The strategies can be incorporated into reactions that involve transamination schemes and/or reductive amination schemes. In the case of transamination, for instance, using transamination to cause ring closure of higher amines in the presence of a suitable catalyst leads to desired cyclic triamines with notable conversion and yield. In the case of reductive amination, reacting suitable polyfunctional precursors in the presence of a suitable catalyst also yields cyclic triamines via ring closure with notable selectivity and conversion. Both transamination and reductive amination methodologies can be practiced under much milder temperatures than are used when solely acid catalysts are used. Preferred embodiments can produce reaction mixtures that are generally free of salt by-products.
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Page/Page column 27-28
(2010/04/28)
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- METHOD FOR PRODUCING ETHYLENEAMINES
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The invention relates to the production ethyleneamines by reacting monoethanolamine (MEOA) with ammonia in the presence of a catalyst inside a reactor (1) and by separating the resulting reaction discharge. During separation, the ethylenediamine (EDA) obtained is reacted inside a separate reactor (2) in the presence of a catalyst to form diethylenetriamine (DETA), and the resulting reaction discharge is fed to the separation of the reaction discharge resulting from the reactor (1).
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Page/Page column 10; 11
(2008/06/13)
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- Formation and Catalytic Hydrogenation of the Dimer of 1,2,3,4,5,7a-Hexahydroimidazopyrazine
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Reaction of diethylenetriamine with glyoxal or N,N'-dicyclohexylethylenediimine forms the novel heterocycle 1,2,3,4,5,7a-hexahydroimidazolpyrazine 1 (R1 + R2 = H) which is isolated as its dimer.Catalytic hydrogenation converts 1 into N-(2-aminoethyl)piperazine in high yield.
- Mirkin, Chad A.,Premecz, Joan E.,Ford, Michael E.,Johnson, Thomas A.
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p. 839 - 840
(2007/10/02)
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- The Reactions of Amine, Polyamine and Amino Alcohol Corrosion Inhibitors in Water at High Temperatures
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A stainless steel reactor has been used to investigate the reactions of mono-, di-, tri- and tetraamines, amino alcohols and amino ethers in degassed aqueous solution at 240-300 deg C.The predominant reactions involved nucleophilic substitutions, where the amino nitrogen acts as the nucleophile, and not solvolyses.With α,ω-diamines, cyclic and bicyclic amines were formed by inter- or intra-molecular processes.Amino alcohols react by displacement of the hydroxy rather than the amino group.The material balance deficit, however, was generally significant, and it issuggested that the missing materials are polyamines arising from polymerisation that competes with cyclisation.The major product from 1,2-diaminoethane and related polyaminoethanes and ethanolamines is diazabicyclooctane.The kinetics of some of the cyclisations were studied.Reactions of α,ω-diamines and 5-aminopentan-1-ol are first order in reactant.Conversion of 1,4-diaminobutane to pyrrolidine occurs with high selectivity at 240 deg C; in contrast the reactions of the less reactive compounds were less selective, probably due to the formation of polymeric materials.The relative reactivity of the substrates is discussed in detail.
- Smith, John R. Lindsay,Smart, Alison U.,Twigg, Martyn V.
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p. 939 - 947
(2007/10/02)
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- REGIOCHEMISTRY AND KINETICS OF CYCLIZATION OF N-(2-CHLOROETHYL)POLYETHYLENEPOLYAMINES
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The directions of competitive intramolecular cyclization of a series of N-(2-chloroethyl)polyethylenepolyamines yielding 3- and 6-member nitrogen-containing heterocycles were investigated.The kinetic characteristics of these reactions were studied.A qualitative scheme for synthesis of polyethylenepolyamines that explains the practically observed characteristics was proposed based on the results obtained and the published data.
- Chechik, V. O.,Bobylev, V. A.,Selivanov, S. I.
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p. 1541 - 1544
(2007/10/02)
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- SYNTHESIS OF AKALI AND HEAVY METAL DITHIO- AND THIOCARBAMATES BASED ON N-(β-AMINOETHYL)PIPERAZINE
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A series of alkali and heavy metal dithio- and thiocarbamates based on N-(β-aminoethyl)piperazine and its derivatives N-(β-piperazinoethyl)imides, N-piperazine, and N-(β-salicylideneaminoethyl)piperazine is prepared.Methods for preparation of dithio- and thiocarbamates based on piperazine are improved.Alkali metal dithio- and thiocarbamates based on piperazines form polymeric complexes with heavy metals.
- Zagidullin, R. N.
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p. 1275 - 1279
(2007/10/02)
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- INTRAMOLECULAR GENERAL-BASE CATALYSIS OF SCHIFF-BASED HYDROLYSIS BY TERTIARY AMINO GROUPS.
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Hydrolysis of a series of Schiff bases derived from benzophenone and various amines has been studied kineticlly in aqueous solution. A linear correlation of the log of the rate constants for the water reaction with the Schiff base pK//a (slope minus 0. 70) shows large positive deviations for Schiff bases derived from (2-aminoethyl)diethylamine, N-(2-aminoethyl)morpholine, N-(2-aminoethyl)piperazine and 2-(aminomethyl)pyridine (1i) but small deviations for Schiff bases from N-(3-aminopropyl)morpholine and 2-(2-aminoethyl)pyridine. The deviations found are attributed to intramolecular general-base catalysis of the water reaction by the internal tertiary amino groups. Magnitudes of the rate enhancement are correlated well with pK//a//l of the internal catalyst ( beta equals 0. 49). Effective concentrations of the internal bases are estimated to range from 340 (1e) to 40 M.
- Okuyama,Shibuya,Fueno
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p. 730 - 736
(2007/10/02)
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- Separation of blood coagulation factors with non-activating polyelectrolytes
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Blood coagulation factors such as Factor VIII are separated from admixture with other blood proteins without producing activation of said coagulation factors by contacting with a water-insoluble, cross-linked polyelectrolyte copolymer of (a) C2-18 unsaturated monomer and (b) C4-12 unsaturated polycarboxylic acid or anhydride which is partially substituted at its free carboxyl or anhydride sites with amine-imides and in which substantially all the remaining free carboxyl or anhydride sites are blocked with alkoxyalkylamine to form alkoxyalkylimide units.
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