- New method for preparing N,N'-dimethylethylenediamine and N,N'-dimethyl-1,3-propanediamine
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The present invention relates to a new method for preparing N,N'-dimethylethylenediamine and N,N'-dimethyl-1,3-propanediamine, wherein 1,3-dimethyl-2-imidazolidinone or 1,3-dimethyl-tetrahydro-2-pyrimidone is used as a raw material, a suitable alkali is added, and a heating ring-opening reaction is perform to prepare N,N'-dimethylethylenediamine and N,N'-dimethyl-1,3-propanediamine. In the prior art, the conventional method performs alkylation by using the amine as the raw material to generate more by-products. According to the present invention, the method completely avoids the problem in theprior art, has characteristics of simple operation, high yield, less three-waste and high product purity, and is suitable for industrial production.
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Paragraph 0015-0020
(2019/10/01)
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- SATURATED N-HETEROCYCLIC CARBENE-LIGAND METAL COMPLEX DERIVATIVES, PREPARING METHOD THEREOF, AND PREPARING METHOD OF SILANE COMPOUND BY HYDROSILYLATION REACTION USING THE SAME AS CATALYST
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Provided are a saturated N-heterocyclic carbene-ligand metal complex derivative, a method for preparing the same, and a method for preparing a silane compound by hydrosilylation using the same as a catalyst. To describe in more detail, the metal complex derivative has a saturated N-heterocyclic carbene derivative and an olefin ligand at the same time. A silane compound is prepared by hydrosilylation in the presence of the metal complex derivative as a catalyst. The provided metal complex derivative of the present invention has superior stability during hydrosilylation reaction and is capable of effectively performing the hydrosilylation reaction at low temperature even with small quantity. Further, a product with superior regioselectivity may be obtained. In addition, after the hydrosilylation reaction is completed, the metal complex derivative may be recovered and recycled.
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Page/Page column 8
(2011/07/08)
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- SATURATED N-HETEROCYCLIC CARBENE-LIGAND METAL COMPLEX DERIVATIVES, PREPARING METHOD THEREOF, AND PREPARING METHOD OF SILANE COMPOUND BY HYDROSILYLATION REACTION USING THE SAME AS CATALYST
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Provided are a saturated N-heterocyclic carbene-ligand metal complex derivative, a method for preparing the same, and a method for preparing a silane compound by hydrosilylation using the same as a catalyst. To describe in more detail, the metal complex derivative has a saturated N-heterocyclic carbene derivative and an olefin ligand at the same time. A silane compound is prepared by hydrosilylation in the presence of the metal complex derivative as a catalyst. The provided metal complex derivative of the present invention has superior stability during hydrosilylation reaction and is capable of effectively performing the hydrosilylation reaction at low temperature even with small quantity. Further, a product with superior regioselectivity may be obtained. In addition, after the hydrosilylation reaction is completed, the metal complex derivative may be recovered and recycled.
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Page/Page column 13
(2011/07/30)
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- Continuous chemoselective methylation of functionalized amines and diols with supercritical methanol over solid acid and acid-base bifunctional catalysts
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The selective N-methylation of bifunctionalized amines with supercritical methanol (scCH3OH) promoted by the conventional solid acids (H-mordenite, β-zeolite, amorphous silica-alumina) and acid-base bifunctional catalysts (Cs-P-Si mixed oxide and γ-alumina) was investigated in a continuous-flow, fixed-bed reactor. The use of scCH 3OH in the reaction of 2-aminoethanol with methanol (amine/CH 3OH = 1/10.8) over the solid catalysts led to a significant improvement in the chemoselectivity of the N-methylation. Among the catalysts examined, the Cs-P-Si mixed oxide provided the most efficient catalyst performance in terms of selectivity and reactivity at 300 °C and 8.2 MPa; the N-methylation selectivity in the products reaching up to 94% at 86% conversion. The present selective methylation was successfully applied to the synthesis of N-methylated amino alcohols and diamines as well as O-methylated ethylene glycol. Noticeably, ethoxyethylamine was less reactive, suggesting that the hydroxy group of the amino alcohols is a crucial structural factor in determining high reactivity and selectivity, possibly because of the tethering effect of another terminus, a hydroxo group, to the catalyst surface. The magic-angle-spinning NMR spectroscopy and X-ray diffraction analysis of the Cs-P-Si mixed oxide catalyst revealed that the acidic and basic sites originate from P2O5/SiO2 and Cs/SiO2, respectively, and the weak acid-base paired sites are attributed to three kinds of cesium phosphates on SiO2. The weak acid-base sites on the catalyst surface might be responsible for the selective dehydrative methylation.
- Oku, Tomoharu,Arita, Yoshitaka,Tsuneki, Hideaki,Ikariya, Takao
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p. 7368 - 7377
(2007/10/03)
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- Episulfide compound, method for producing the same and optical product comprising the same
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The invention relates to a novel episulfide compound useful as a starting material for optical materials that have a high refractive index and a high Abbe's number and to provide a method for efficiently producing the same and an optical product comprising the same. The episulfide compound represented by the general formula (1) : wherein EP represents and n is an integer of from 0 to 2, and the method for producing the episulfide compound represented by the general formula (1) comprises reacting a mercapto group-having episulfide compound with 2,4,6-trimethylene-1,3,5-trithiane.
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- Sodium channel drugs and uses
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The compounds of this invention comprise 2-10 ligands covalently connected, each of the ligands being capable of binding to a ligand binding site in a Na+channel, thereby modulating the biological activities thereof.
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- Ureas and amides as dipolar aprotic solvents in highly basic media. The dependence of kinetic basicity on solvent composition
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The basicity of dipolar aprotic solvent water HO systems with amides and ureas as the organic component has been studied kinetically because previous information is not available. excluding some H values measured for aqueous dimethylformamide (DMF) and tetramethylurea (TMU). It was found that the increase in basicity with the mole fraction of organic component is at least of the same magnitude as in aqueous dimethyl sulfoxide (DMSO). For instance, in the detritiation of chloroform-t the slopes of the plots log(k2/mol 1 dm3 s 1) vs. x(urea) varied between 11.4 14.6 (as compared to 11.0 in aqueous DMSO) when TMU and cyclic ureas. 1.3-dimethylimidazolidin-2-one (DMI) and 1.3-dimethyl-3.4.5.6-tetrahydropyrimidin-2(1H)-one (DMPU). were used as the organic component in solvent mixture. In aqueous TMU acidity functions H were extrapolated from kinetic results using linear free energy correlations. Agreement with literature values was evident. This method was also used to extrapolate the H values in aqueous DMPU. On the basis of present work aqueous ureas can be recommended as solvents in highly basic media. The utility of amides. dimethylformamide and dimethylacetamide. is limited by their instability in basic water solutions.
- Kankaanperae, Alpo,Scharlin, Pirketta,Kuusisto, Ilona,Kallio, Riitta,Bernoulli, Emma
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p. 169 - 174
(2007/10/03)
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- Linear oligomeric polychelant compounds
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Linear oligomer polychelant compounds and chelates formed therewith have alternating chelant and linker moieties bound together by amide or ester moieties. The compounds have between 3 and 100 chelant moieties, at least one of which complexes a paramagnetic metal ion. The polychelants and especially their paramagnetic metal polychelates are particularly suitable for diagnostic imaging.
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- Condensation of Alkanediamines with Formaldehyde; Intramolecular Disproportionation of N-Hydroxymethyl Groups into N-Methyl and N-Formyl Groups
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The condensation of α,ω-alkanediamines NH2(CN2)nNH2 with aqueous formaldehyde has been studied by NMR spectroscopy of isolated products and of product mixtures.The condensation was reversible and gave products of widely different types depending on alkane chain length: bicyclic oxadiaza compounds (n = 2, 3, 4), a tricyclic tetraaza compound (n = 2), a quinquecyclic octaaza compound (n = 3), two-dimensional polymers (n = 4, 5).A slow irreversible rearrangement gave in two cases (n = 3, 4), unicyclic 1-formyl-3-methyl-1,3-diaza compounds.The condensation of N,N'-dimethyl-α,ω-alkandediamines CH3NH(CH2)nNHCH3 with aqueous formaldehyde was also studied.The reversible formation of simple unicyclic diaza compounds was observed in all cases (n = 2, 3, 4), but in one case (n = 2) there was again a slow irreversible rearrangement to the N-formyl-N,N'N'-trimethyl derivative.The rearrangement reaction involves a hydride shift and is strictly intramolecular.The conditions for its occurrence can be understood on a conformational basis.
- Dale, Johannes,Sigvartsen, Turid
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p. 1064 - 1070
(2007/10/02)
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