Method for the reductive methylation of primary amines

C - Chemistry – Metallurgy – 07 – C

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260/607.2

C07C 209/68 (2006.01) C07C 209/26 (2006.01) C07C 211/14 (2006.01)

Patent

CA 2005892

ABSTRACT A process for the preparation of permethylated amines, particularly pentamethyldiethylenetriamine, by the reductive methylation of diethylenetriamine in the presence of hydrogen, a nickel-containing catalyst, aqueous formaldehyde and methanol, comprising feeding continuously the formaldehyde to the reaction system in two phases. In the first phase, a sufficient amount of formaldehyde to mono-methylate the primary amine groups present, is fed to the reaction system at a high flow rate, and thereafter the flow rate of the formaldehyde is substantially reduced, for the reductive methylation of the secondary amine groups. By this method the pro- duction of by-products is substantially reduced and preparation times are significantly shorter in compar- ison to processes where the formaldehyde flow rate remains constantly high for the entirety of the reaction.

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