Removing dimethylamine.HCl with rxtal...

[raffike]

Now raf ran another AmCl+HCHO-->MeAmCl.HCl reaction and is wondering if dimethylamine.HCl could be removed with denat alcohol rxtal.Raf has noticed that reaction itself is pretty exothermic and this time temp also reached 108-109 during the peak(at 80C it kicks in and is pretty violent with temperature rising).Some air cooling was applied without much success but temp didn't rise over 110 so raf thinks there's no problem.But raf thinks there is still a significant dimethylamine.HCl content-some sources even claim upto 20% dimethylamine.HCl content with this reaction.Raf thinks dimethylamine could be removed with with careful rxtal and some bees tell this works.Raf thinks that methylamine.HCl is less soluble in alcohol than dimethylamine.HCl.Would one rxtal cut down the content of dimethylamine.HCl to <3%?

[Organikum]

Chloroform is the only relieable way to remove the dimethylamine. Making chloroform is one of the most easy synths on Rhodiums page for sure, but not my favorite one. But do it once big, blow a day on it and you will have enough chloroform to wash your methylamine for a long time and it will be enough left for the dark side of your personality to do evil things at night. ( Ya know...the virgin...the handkerchief..the chloroform bottle...a hand in leathergloves....dramatic music....)

Acetone works also to wash out the dimethylamine but sadly only in some parts of Canada whilst crossing a lake in a canoo. Or something like this.  

Separation by recrystalisation is possible - not only in Canada, but seen realistic nobody of us two will get halfway pure methylamine this way. I know it for me as my shit always crystallizes when I am pissing or so. I guess it for you by your tendency to boil things over - no offense intended, you see I read your posts  

[raffike]

Why wouldn't recrystallisation work to remove dimethylamine.Dimethylamine and methylamine have very different physical properties when it comes to solubility.Ammonium chloride is very little soluble in alcohol,methylamine a bit more and dimethylamine should most soluble.Raf could buy some chloroform but he's very short on cash at the moment.6 kgs of chloroform costs around 40 bucks over but he doesn't have that much,maybe next week.In one doc at rhodium somebody suggests alcohol recrystallization to remove dimethylamine.Well at least it can't hurt,can it?

[hCiLdOdUeDn]

https://www.thevespiary.org/rhodium/Rhodium/chemistry/methylamine.html

Havent you read the methylamine synthesis FAQ? Recrystallization is the essential procedure in purifying the Ammonium Chloride/Methylamine.HCl/Diethylamine.HCl mixture. The procedure is explained in there well.

Also havent you heard of better ideas on producing methylamine without the worry of contamination of diethylamine? Try the al/hg reduction of just nitromethane alone. Then add NaOH to the post reduction solution and then bubble the methylamine gas into ethanol.

Post 383107

(Osmium: "Finally someone is doing this MeNO2 prereduction.", Methods Discourse)

Synthesis of Chloroform is really easy. All you need as acetone and calcium hypochlorite.

https://www.thevespiary.org/rhodium/Rhodium/chemistry/chloroform.html

Good luck~

[raffike]

Mhh...raf got about 60 grams of recrystallized stuff.He should have got about 300-350.He saved all that denatured stuff used,will reduce volume to 1/2 and see if more comes out.He used 1,5 liters of denatured to rextal 300-400 grams,is that too much?He thinks so.Crystals itself are pure white plates or something,i don't know how you call em.

[GOD]

they are scaley- kind of like white, wet-looking, semi-opaque micca.  Kind of crunchy- makes you wanna pour some milk on 'em and have a spoonful.

mmmmmmmm!!! Love that smell    

swim had a stink on him like nobodies buisness!  He went to the grocery store after accidentally touching a little peice, you should have seen the dirty looks

[raffike]

Reduced volume to 600 mls and chilled,harvested another 100 grams and washed with some DCM to get em dry.Overall yield around 170 or so grams which means that denat rextal is pretty low yielding.It gave very good quality product thouhg.Will stick to chloroform/acetone wash next time.Little ammonium chloride won't do any harm as it forms very unstable imines and methylamine will easily push it out of playground.

PS raf has been to school day after dreaming some methylamine.People wonder where does the rotten fish smell come from.Luckily they don't raf is reeking it sometimes.It takes so little methylamine to make so much stink,even if you wash hands many times,it might be still with ya.

[Chromic]

Either acetone or dichloromethane will work to remove dimethylamine hydrochloride.

[raffike]

How do you know that?How much acetone is needed to remove most dimethylamine.HCl?

[Organikum]

but Organic Synthesis and VOGEL recommend chloroform for removing dimethylamine.HCl. So this may be regarded as a doubtless working way. About the usability of acetone or DCM there are different opinions present.
With chloroform you are on the safe side.
I am not sure about DCM, acetone was told NOT to be useful for this purpose. (probably this is just another conspiracy - the chloroform gang   )

This is for purposes of documentation and information on the existance of differing opinions solely and it´s not intended to start the hassle again!

[raffike]

But how about ordering some from Aldrich or like and testing it out.Raf could do it,it's not watched nor expensive chem and 100 grams would be enuff for all solubility tests.

[Rhodium]

That would be excellent if you could do that - bees making empirical experiments to help others are ALWAYS welcome!