- Synthesis method of 2,2'-diamido-N-methyldiethylamine
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The invention discloses a synthesis method of 2,2'-diamido-N-methyldiethylamine. The synthesis method is characterized in that acetic anhydride is added dropwise into N-methyldiethanolamine, ripeningis conducted after dropping dropwise adding is completed, and a compound II is obtained; phthalimide is added into the compound II, heating and ripening are conducted after adding is completed, and acompound III is obtained; 6N hydrochloric acid is added into the compound III, then heating and ripening are conducted after adding is completed, and a compound IV is obtained; and sodium methoxide isadded into the compound IV, and ripening at the low temperature is conducted after adding is completed. The technological method for synthesizing high-purity 2,2'-diamido-N-methyldiethylamine has theadvantages of being low in cost, high in yield, simple in purification technology, convenient to operate and suitable for industrialized production, the GC purity of the prepared 2,2'-diamido-N-methyldiethylamine can be as high as 99% or above, and the total yield is 60% or above.
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Paragraph 0042; 0043; 0044; 0045; 0046; 0047
(2019/03/28)
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- N-methyl piperazine a process for the preparation of (by machine translation)
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The invention relates to a preparation method of N-methyl piperazine. The preparation method comprises the following steps: (1) carrying out reaction on iminodiacetonitrile (IDAN) and methanal under the acidic condition to prepare N-methyl iminodiacetonitrile; and (2) carrying out hydrogenation reaction on N-methyl iminodiacetonitrile at the temperature of 70-140 DEG C and the pressure of 2-8MPa, wherein a molecular-sieve modified zirconium-based superacid serves a carrier, and one or two or more of the active metals of Fe, Co, Ni, Ru and Rh serves/serve as a hydrogenation catalyst. Compared with the prior art, the preparation method provided by the invention has the advantages of high yield due to the adoption of the catalyst and low equipment investment. In addition, the raw materials for preparing the N-methyl piperazine are low in cost and are easy to obtain.
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Paragraph 0066-0074
(2019/02/02)
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- SYNTHESE DE SPERMINE ET DE SPERMIDINE SELECTIVEMENT SUBSTITUEES SUR LES FONCTIONS AMINES SECONDAIRES
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Protection of the primary amino group of various polyamines followed by alkylation or benzoylation at the secondary amino group and finally removal of the protecting group leads to the N-methyl (23, Scheme 3), N-benzoyl (11, Scheme 1) (ethylenetriamine, N-benzoyl spermidine (22, Scheme 3), N,N'-methyl (27, Scheme 4)-ethyl (28, Scheme 4), -propyl (16, Scheme 2) -benzoyl (15, Scheme 2) spermine.
- Garrigues, Bernard,Vidaud, Lionel
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p. 775 - 786
(2007/10/02)
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- Chemistry of Nitrogen Mustard studied by Nuclear Magnetic Resonance Spectroscopy
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Reactions of the nitrogen mustard drug 2-chloro-N-(2-chloroethyl)-N-methylethanamine with nucleophiles in aqueous solution have been studied by 1H and 13C n.m.r. spectroscopy.Conditions have been devised for converting the mustard into the N-2-chloroethyl-N-methylaziridinium ion which has been characterized by 1H n.m.r. spectroscopy.To assist the studies of reactions of the mustard by 13C n.m.r. spectroscopy, it has been prepared labelled at both C-2 atoms by 13C.It is shown that reactions of the mustard with strong nucleophiles (e.g. thiosulphate) proceed to a product of disubstitution, without the aziridinium ion being detected spectroscopically, although its intermediacy is inferred by examining the distribution of 13C in product from 13C-labelled mustard.Less reactive nucleophiles (e.g. thiourea) yield a product of disubstitution via spectroscopically detected intermediates (aziridinium ion and monosubstituted intermediate).Relatively weak nucleophiles (e.g. guanosine) did not give detectable products of substitution; cis- and trans-NN'-2-chloroethyl-NN'-methylpiperazinium dichloride were formed via the aziridinium ion.The reaction of the mustard with excess of ammonia gives a 3 : 2 ratio of 2-amino-N-(2-aminoethyl)-N-methylethanamine and N-methylpiperazine.The distribution of 13C label in these products derived from 13C-labelled drug shows that the triamine is formed via aziridinium intermediates, whilst the piperazine arises via intramolecular cyclisation of the intermediate 2-amino-N-(2-chloroethyl)-N-methylethanamine.
- Golding, Bernard T.,Kebbell, Michael J.,Lockhart, Ian M.
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p. 705 - 714
(2007/10/02)
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