Author Topic: MeNH2 gas from MeNH2.HCl using NaOH  (Read 2758 times)

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r2e3

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MeNH2 gas from MeNH2.HCl using NaOH
« on: April 27, 2004, 02:32:00 PM »
Swim has the necessary precursors required for 'alkyl reduction' in the synthesis of MDMA but needs clarification on how to actually generate the methylamine gas before dissoving it in ice cold methanol.
He realises that it's a reaction with NaOH but does this involve a saturated aqueous solution and the MeNH2 crystals?
He believes that water can take up plenty of methylamine - will this cause wastage? The universal guides provided are not very clear with respect to this step so any pointers would be appreciated.

r2e3

pooky

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Pooky's Freebaser
« Reply #1 on: April 30, 2004, 05:47:00 PM »
This is such an easy thing to do,once you know.P doesn't want you to kill yourself..this may be the possibly the safest way.
P has a garden sprayer,in which is concentrated NaOH.A new outfeed hose,made from  clear 1/2 inch PE tubing goes into another sprayer's outfeed line,and this number 2 sprayer  has MeNH2.HClin it.Now this second sprayer,from it's overpressure valve port (valve removed) has a line (outfeed for the gas)going into another sprayer (the same idea as number 2 sprayer) but  number 3 has a hose running from the infeed to the bottom of the sprayer.This is filled with CaCl2 to dry the gas.
From this outfeed (the removed pressure valve again) a hose runs to the cooler.
Next is a white 8 inch diameter pipe,the type for water or sewer lines,the bottom properly epoxied with  the proper cap-about 1 meter tall.Inside this is a glass tube just over 1 meter long (from a neon sign shop)exiting from the bottom (and sealed with epoxies and sealers)and exiting through an unglued top.The glass tube is supported at the top.P's freezer goes to -30 C,and the plastic pipe is  filled with a supercooled brine solution.

Pump a little on the first sprayer,NaOH moves up the tube and hose,drips (into number2)onto the MeNH2 which forms a gas.Next it goes out the tube and down into the bottom of number 3 to rise up and be dried through the CaCL2.Next it goes down through the glass tube in the supercooled brine and condenses to the freebase form.This oozes out into a short hose into a flask in a container with more brine and some supercooled methanol.Weigh everything first so you know what you have.
Between number one and 2,P has a T valve from a hydroponics store-the normal flow goes straight through the T,and P has another pressurized sprayer,in order to purge the leftover gas in number 2 through the freebaser when it is all done.Just so you dont get gassed when opening it all up,P can also uses water after the air purge.
Also P has a cheap vacuum gauge on number 2 to let him know when she is starting to suck back,then P gives her another little shot of NaOH.
P is a visual person,and all this may sound complicated,but just buy all the sprayers(must have a removable over pressure valve)some hose and tubes and some epoxy and get at it.It may cost$150,but is worth it.
P messed around with horse syringes with NaOH in them into containers with the amine , and into ice cold MeOH but the gas is too hot (P guesses)and 90% just bubbles right through the MeOH,regardless of stirring.
Epoxy and clamp every hose,seal any possible gas leaks with great fervor.In 2 and 3 P chopped off the air pump and epoxied a seal onto what was left.They still screw in and out with the chopped off handle.
Resist the temptation to make more than what you need.P got greedy one day and made a "bit much" to be stored in the freezer and....the power went out.The freebase vaporized at -6C or whatever and blew the container to pieces.The freezer and area was not in the home by design,but this  saved P's neck.
Remember this stuff is damn nasty and deadly poisonous,and be very careful.Don't do it in the house or near neighbours-and if things start hissing,don't be afraid to run for it!In fact, P does not recommend you try this at all.

pooky

  • Guest
Safe and quick
« Reply #2 on: May 01, 2004, 09:52:00 PM »
It takes an half an hour to build,a day for the epoxies to set-and P has never gotten a blast of gas in the face after building this.And P could make a kilo of freebase MeNH2 in about 30 minutes...take it or leave it ;)
PS:the bottom drip tube must be submerged in the MeOH,in case a little gas gets through.And the hose to the glass tube is forced on and not glued;so when you are done, some MeOH can be run through the tube to flush any frozen base out.Just take her easy..

pooky

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P will find a way to break it..
« Reply #3 on: May 04, 2004, 01:18:00 PM »
P did something similar to this,but with a 2 necked flask,addition funnel on one neck and the 3 way and 2  condensors in series on the other.
It worked OK but P's jacket caught the vacuum fitting and P pulled the fuc%er over while in full gassing mode-had to run for it while $600 worth of glass smashed to pieces and a mushroom cloud filled the garage.
Is funny now but P was not too impressed at the time...

r2e3

  • Guest
detail..
« Reply #4 on: May 07, 2004, 11:44:00 AM »
thanks for the responses :-)
kinda had a learning experience...
got greedy - doh -  and didnt stop at 15g in solution (50g MDP) and..  suck back sucks.
shoulda just gone for the MDA route - nice and easy
i will check out the alternatives you have suggested
will study your descriptions after a bit of r n r
cheers

pooky

  • Guest
oops P screwed up
« Reply #5 on: May 10, 2004, 08:43:00 PM »
P was tired(driving 7 hours) when posting the second time,confused gasser with freebaser,and posted wrong.Got it all screwed up.But P usesthe same apparatus for both.
In freebaser,#1 has lye,#2 has MeNH2,#3 has CaCl2 and goes  through chiller into room temperature stirring MeOH..can get over 100 g in 10 minutes,with proper venting very little smell.
When gassing #1 has the 33% HCl,#2 the sulphuric acid (drain cleaner),#3 has the CaCl2 and this goes throught the chiller to the cooled freebase/acetone.That is the kilo in half an hour.
So sorry, hope no trouble caused,P

r2e3

  • Guest
ok
« Reply #6 on: May 18, 2004, 06:43:00 PM »

terbium

  • Guest
Methylamine gas
« Reply #7 on: May 20, 2004, 11:36:00 PM »
I suggest putting NaOH pellets into a flask and dropping a saturated, aqueous solution of MeAm.HCl onto the pellets.


psytech

  • Guest
methylamine naoh meoh
« Reply #8 on: May 21, 2004, 02:45:00 PM »
if you need a 10% meam sol.in meoh, just (dissolve) x moles naoh in 1/2 volume meoh, then chill, add x mole meam to 1/2 volume meoh chill, combine slowly, cooling with ice salt bath, filter and dry with favorite agent.

OcoteaCymbarum

  • Guest
A suggestion that makes a lot of sense
« Reply #9 on: May 22, 2004, 06:52:00 AM »
Good thinking!
I was about to build a similar setup to pooky but your idea of dropping aqueous meam is genius!
That way, you dont loose any methylamine, you use only what is required and you keep the solution for latter use!
The other way around, you would have to guess just about how much meam you need, and therefore loose some everytime!
Thanks Terbium
OC

pooky

  • Guest
Yes
« Reply #10 on: May 22, 2004, 11:08:00 AM »
Dripping the MeNH2 onto the pellets works fabulously,but be sure you can get a long screwdriver into your (unbreakable)reaction vessel,as the NaOH almost turns to stone..

r2e3

  • Guest
info
« Reply #11 on: May 28, 2004, 10:20:00 AM »
great!

When R2 did this the MeAm was a concentrated aq solution and it was dropped onto powder form NaOH. It did work well -lots of gas was generated. How much was MeAm R2 does not know...

Should the gas be dried over CaCl2 or NaOH before passing into MeOH? (Plenty water vapour genereated by the reaction of the 2 - not endothermic as stated in the literature) Have silica gel in main reaction mixture.

Also  - silica beads seem to soak up the MeAm gas. Should prolonged exposure be avoided? R2 must have used about 150g of MeAm and got zilch in the way of product. Minimal loss occured during gassing. 

Saw lotsa bubbles - no smell and no real net increase in MeOH solution weight..? Odd The actual solution stank to high heaven. Can you over gas the MeOH? ie what is the max that can be dissolved into MeOH (per 100ml for eg)

Any other hints would be handy ;-)

zero_nrg

  • Guest
Previous posts indicate that methanol will max
« Reply #12 on: May 28, 2004, 12:16:00 PM »
Previous posts indicate that methanol will max out at about 10% methylamine (cold MeOH).  I believe 100 ml MeOH (density ,791) will hold approx. 8.77 grams of methylamine.  The first time swim tried to gas MeOH he made the mistake of putting powdered CaCl2 in the condenser attatched directly to the reaction flask.  It caked and clogged and was quickly removed and the gas bubbled directly out of the reaction flask into the cold MeOH (better to put the drying tube on top of the primary condensing condenser).  Btw there were a hell of a lot of bubbles.  The MeOH was dried with silica gel and used in the LT anhydrous procedure where yields were nearly quantitative. Also, I don´t believe silica gel "soaks up" methylamine gas.  Silica gel soaks up water which may contain methylamine gas. Overgassing MeOH (adding more Meam gas than it can dissolve) results in waste as the gas simply wont dissolve in the alcohol and stinks up the room. Approx. how much water did you use to make the saturated soln. with 150 gr. methylamine HCl .?

zero_nrg

  • Guest
This method was tried using 100 gr.
« Reply #13 on: May 30, 2004, 02:18:00 PM »
The Terbium method was tried using 100 gr. methylamine HCl (1.48 mol?).  The Methylamine HCl was put into an addition funnel and dissolved in a minimum amt. of water (actually still a few crystals floating around in it. The add´n funnel connected to 3 neck flask containing 80 gr. (2 moles) NaOH.  A 400mm condenser was attatched (vertically of course) and a drying tube on top of that.  An anti-suckback flask was placed between the reaction set-up and the 514 gr. (excess)cold methanol in an ice bath.  The reaction flask was swirled by hand every now and then.  The methanol weighed 553.81 grams after reaction for a gain of 38.98 gr. freebase which is almost 85% assuming that Meam HCL has a MW of 67.52 (I calculated that meam gas mw =31.06 + HCl mw = 36.46).  Added a little more water and NaOH after all methylamine HCl was added and that seemed to generate a little more gas.  Beware of suck-back. Never had yield this high before. -zero

terbium

  • Guest
Acidic drying agents.
« Reply #14 on: June 02, 2004, 07:25:00 PM »

Also, I don´t believe silica gel "soaks up" methylamine gas



Calcium chloride will definitely absorb the methylamine or any amine. I would be wary of silica also. NaOH pellets would be best for drying methylamine gas. Bubbling the methylamine gas through a saturated NaOH solution should also work. You can even get away without any drying if you let the gas cool through a long neck flask or reflux condensor.