- Method for preparing pentamethyldipropylene triamine
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The invention provides a method for preparing pentamethyldipropylene triamine. The method comprises the following steps: (1) performing a reaction on 3-dimethylaminopropylamine and acrylonitrile so asto form a 3-[[3-(dimethylamino)propyl]amino]propionitrile reaction solution, and performing separation so as to obtain a 3-[[3-((dimethylamino)propyl]amino]propionitrile pure product; (2) performinga hydrogenation reaction on 3-[[3-(dimethylamino)propyl]amino]propionitrile, hydrogen and a solvent under the action of a catalyst so as to obtain a N'-(3-aminopropyl)-N,N-dimethyl-1,3-propylene diamine reaction solution; and (3) performing a methylation reaction on the N'-(3-aminopropyl)-N,N-dimethyl-1,3-propylene diamine reaction solution obtained in the step (2), formaldehyde and hydrogen underthe action of a catalyst so as to obtain pentamethyldipropylene triamine. The method has the advantages of cheap and easily available starting materials, good selectivity to the product and high product yield, and the method is economical and effective, and has industrialization prospects.
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Paragraph 0065; 0068; 0070; 0072; 0075; 0077; 0079; 0082
(2019/11/20)
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- An efficient synthesis of N,N,N′,N′,N″-pentamethyldipropylenetriamine
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N,N,N′,N′,N″-Pentamethyldipropylenetriamine (PMDPTA) has for a long time been employed as an efficient catalyst in the production of polyurethane materials. A green and effective synthetic route to PMDPTA was successfully established from experiments described in this paper. PMDPTA was obtained from methylamine, acrylonitrile and formaldehyde via a Michael addition, catalytic hydrogenation and methylation in 65% overall yield. Furthermore, methanol was employed as the only solvent in all of the three steps, resulting in the convenient recovery of methanol. This route is thus suitable for industrial production.
- Gui, Sizhe,Mu, Manman,Luo, Hao,Liu, Na,Shen, Huawei,Chen, Ligong
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p. 486 - 488
(2016/08/13)
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- Contrasting copper-dioxygen chemistry arising from alike tridentate alkyltriamine copper(I) complexes
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Copper(I)-dioxygen interactions are of great interest due to their role in biological O2-processing as well as their importance in industrial oxidation processes. We describe here the study of systems which lead to new insights concerning the factors which govern Cu(II)-μ-η2:η2 (side-on) peroxo versus Cu(III)-bis-μ-oxo species formation. Drastic differences in O2-reactivity of Cu(I) complexes which differ only by a single -CH3 versus -H substituent on the central amine of the tridentate ligands employed are observed. [Cu(MeAN)]B(C6F5)4 (1) (MeAN = N,N,N′,N′,N′-pentamethyl-dipropylenetriamine) reacts with O2 at -80 °C to form almost exclusively the side-on peroxo complex [{CuII(MeAN)}2(O2)]2+ (3) in CH2Cl2, tetrahydrofuran, acetone, and diethyl ether solvents, as characterized by UV-vis and resonance Raman spectroscopies. In sharp contrast, [Cu(AN)]B(C6F5)4 (2) (AN = 3, 3′-iminobis(N,N-dimethyl-propylamine) can support either Cu2O2 structures in a strongly solvent-dependent manner. Extreme behavior is observed in CH2Cl2 solvent, where 1 reacts with O2 giving 3, while 2 forms exclusively the bis-μ-oxo species [{CuIII(AN)}2(O)2]2+ (4Oxo). Stopped-flow kinetics measurements also reveal significant variations in the oxygenation reactions of 1 versus 2, including the observations that 4Oxo forms much faster than does 3; the former decomposes quickly, while the latter is quite stable at 193 K. The solvent-dependence of the bis-μ-oxo versus side-on peroxo preference observed for 2 is opposite to that reported for other known copper(I) complexes; the factors which may be responsible for the unusual behavior of 1/O2 versus 2/O2 (possibly N-H hydrogen bonding in the AN chemistry) are suggested. The factors which affect bis-μ-oxo versus side-on peroxo formation continue to be of interest. Copyright
- Liang, Hong-Chang,Zhang, Christiana Xin,Henson, Mark J.,Sommer, Roger D.,Hatwell, Karen R.,Kaderli, Susan,Zuberbuehler, Andreas D.,Rheingold, Arnold L.,Solomon, Edward I.,Karlin, Kenneth D.
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p. 4170 - 4171
(2007/10/03)
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- Fragmentation During the Formic Acid/Formaldehyde (Eschweiler-Clarke) Methylation of Polyamines
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Eschweiler-Clarke methylations of both acyclic and cyclic polyamines can lead to methylation products of fragments of the original polyamine; thus 1,5,9,13-tetra-azatridecane yields 1,1,3,3-tetramethylpropanediamine exclusively and 1,5,9-triazacyclododecane gives 45 percent 1,5,9-trimethyl-1,5,9-triazacyclododecane and 45 percent 2,6,10-trimethyl-2,6,10-triazaundecane.
- Alder, Roger W.,Colclough, David,Mowlam, Rodney W.
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p. 7755 - 7758
(2007/10/02)
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