Read these docs, I think you might get some guidance from there, as I think they concern the same compounds, but with a different nomenclature:
Post 414873 (https://www.thevespiary.org/talk/index.php?topic=12648.msg41487300#msg41487300)
(Rhodium: "Cyclic Methyleneamines. Part I.", Tryptamine Chemistry)
Post 415886 (https://www.thevespiary.org/talk/index.php?topic=12648.msg41588600#msg41588600)
(Rhodium: "Cyclic Methyleneamines. Part II.", Tryptamine Chemistry)
Thanks Rhodium, that was very helpful! Here's what makes me feel better:
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Reduction of Trimethyltrimethylenetriamine
The base was prepared by the slow addition to an ice-cold solution of methylamine (100 parts of 33%) of an ice-cold solution of formaldehyde (70 parts of 40%). It separated as an oily upper layer on addition of stick potash, the solution being cooled in ice. After 48 hours the layer was removed and distilled (bp 166°C) over barium oxide. Yield, 80% of the theoretical.
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So, these compounds can be distilled under normal pressure, and all I have to do to avoid decomposition is keep it away from an acid.
Btw, what's "stick" potash? What form of KOH is that?
Did I find an error in the following synth:
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Tri-n-butyltrimethylenetriamine
This was prepared from n-butylaniline (20g) and 40% formaldehyde (21g) in the cold. The oily base, dried over barium oxide for 2 days, had bp 285°C and d17° 0.8550.
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Don't they mean to say n-butylamine instead of n-butylaniline?
Here's my last question, then I'll shut up: Could I make triammoniumtrimethylenetriamine from ammonia/formaldehyde, then heat it with a-methylstyrene, acetic acid/anhydride, like in Patent US2765315 (http://l2.espacenet.com/dips/viewer?PN=US2765315&CY=gb&LG=en&DB=EPD)
to make a prodine. What would be the name of this creation? Any reason why ammonia wouldn't work when plugged into a synth in that patent?
Thanks again! 8)