dormouse (Member)
04-22-00 09:08
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      Methylamine via hoffman -Molly Heart  Bookmark   


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Molly Heart
Member   posted 02-02-99 03:55 PM          
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Please anyone...help me here. I am stuck in a nightmare. I have been unable to get ANY product off the hypohalite hoffman prep for Methylamine! I need the salt BUT the directions seem a little on the lite side. What is the whole "bubbler" thing about? How do I capture the gas? Also, what do I do with the distillate from the reaction, do I use it? It states "Evaporate the bubbler soln. to dryness... HOW? and is the bubbler solution what contains the Meam HCL? THEN..."add 15ml dh2o..." Add it to what soln? I am oh so confused from the ravages of this nightmare! I am almost there I AM a virgin and DO want this so...
 
equarius
Member   posted 02-03-99 01:30 AM          
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It's your lucky day as it looks like Spiceboy has been experimenting and improving this process, check out his recent posts. I read about and even acquired the glassware for this reaction but it sounds too complicated, difficult, and impracticle when compared to the formaldehyde / ammonia (in their many many otc forms) reaction.
 
Molly Heart
Member   posted 02-03-99 10:43 AM          
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Yes, Yes this I know However...I'm at the cusp I tell you, THE CUSP! I already have the acetamide and all. But does anyone think it more beneficial to change methods completely? If so, we are looking at some time b/c I don't have Form. or the ammonium chloride. Please I need tips here. Any and all appreciated!
 
Molly Heart
Member   posted 02-03-99 10:44 AM          
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Yes, Yes this I know However...I'm at the cusp I tell you, THE CUSP! I already have the acetamide and all. But does anyone think it more beneficial to change methods completely? If so, we are looking at some time b/c I don't have Form. or the ammonium chloride. Please I need tips here. Any and all appreciated!
 
spiceboy
Member   posted 02-03-99 02:57 PM          
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Molly- I saw your request in the other thread, so, here goes;
a) The procedure, when done correctly, produces some extremely clean CH3NH2(methylamine).

b) you asked: "what is the whole bubbler thing about?"

Its like this, ok?

When you are doing it via Eleusis' instructions, and you are forming the HALOAMIDE, (this is adding the cold acetamide to the cold hypochlorite and stirring)
you are forming an INTERMEDIATE,in other words, you have made what eventually becomes your goodies, but only halfway,so far.

If you'll notice, Eleusis says to allow the HALOAMIDE to stand a couple of hours.
IMHO, its best to give that shit about4-6 hrs in the freezer, COVERED. Make sure ice doesn't form on your stuff.Apparently, the haloamide CONTINUES to form while standing for some time. Beware! CHLORINE gas is/can be
produced while forming the haloamide. The stuff is as E says, greenish upon chilling.

c) when you take your stuff out of the freezer, you dump the required amount of NaOH into it w/ stirring and it turns milky white.

NOW....partition your milky mixture into an appropriately sized RB flask w/ glass joints.
you DO NOT want it over 2/3 full. Drop a stirbar in. WARNING: Do NOT attempt this without good magstirring. The bumping is incredible, because of localized superheating.(translation: this shit is thick and behaves funny)

After setting up your apparatus for distilling, slowly heat the stuff up to ~63 degrees, and it will go on to 65-67 by itself, and if you're lucky, it will climb up into the 75 area. It re-arranges here, meaning that THIS is where your stuff is actually being made. IT IS A GAS, AS OF NOW.

This is what the bubbler is about. The gas will come off of the glop @ ~50 degrees.
you need to catch the gas in water.I use an erlenmeyer w/ a 2-hole stopper, a 1-way valve and a glass-tipped medicine dropper as my setup, with a bleed-off line into ANOTHER, smaller erlenmeyer to catch what the first one missed.(with me so far?)

It doesn't take much water to catch the vapors, and too much is better than not enough. (water)

BUT!

Soon, you'll find that the temp climbs to 100 deg. and the water starts coming over, and this water contains methylamine TOO....

at the end, I just neutralize the basic water w/ HCL to as close to ph 7 as possible.

That other crap you're confused about is where E describes his way of eliminating NH4Cl as NH3(which is a gas) leaving the extra H and the Cl to convert the product to the salt. I NEVER do that.

Just neutralize it, then EXTRACT the CH3NH2 using denatured alcohol, as CHemHack reccommends.

Hope this helps, but this is a very demanding process for a beginner, as you are required to SYNTHESIZE various aspects of O-chem theory into a viable end result.

GOOD LUCK!


Molly Heart
Member   posted 02-06-99 10:36 AM          
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OH SPICEBOY!!!!!!!!!!!!!! You hope that helps? You are amazing, articulate to boot. You should be writing a book or teaching somewhere...100 THANKS! They say a good deed gets passed along (what goes around comes around) hope I can help someone on the down line. This is what its all about. THE WAR IS OVER! Best of luck your way...
 
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