Author Topic: crystalization...?  (Read 2667 times)

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dave1234

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crystalization...?
« on: July 29, 2004, 02:56:00 AM »
Please help… now for weeks I’ve been going insane, racking my brain at the easiest stage.
I am nearly 100% certain that I should have pure MDMA free base although I can’t crystallize my product, after trying a number of times!

 I have been using the HCI bubbler/generator method from Strike’s TS II.  I have tried using xylene with no success, then redistilling the product I retried with DCM ( also with fresh freebase), and still the same result…nothing. The color seems to be the correct and my AlHg/MeNO seems to have no problems.  Before this I crystallized my MD-P2P using the ‘bisulfate method’ (it wouldn’t crystallize without an added solvent…I’m not sure whether this is a problem?) to get what looked like funny fine yellowish ‘chicken fat’ crystal’s (maybe here this isn’t the correct appearance).  I don’t know where to turn. 

Even with one attempt I put some Ether in the flask to rinse out the product and instantly funny transparent crystals formed on the side of the flask, I believe this happened because there was a small amount of HCI gas held in the product from the previous crystallization attempt. 

My freebase/solvent turns a dark orange after about 10minutes of trying to crystallize.  Sometimes crystallizes start to appear but then disappear , I figure that must be due to the heat…?

Is there any thing I could be doing wrong in crystallization process? Under anhydrous conditions. 

Does the ratio of solvent to freebase matter?
What temperature should the solvent/freebase be at and the HCI?
If all or some of the freebase hasn’t changed from MD-P2P to MDMA will it still crystallize?
Does the ph of the FB make a difference?
What is over or under gassing?
Is there any other process that might work?
Is there any definite way of identifying is the freebase is MDMA?

Without a crystal ball I know it’s hard but please any help will be so much appreciated.
Sorry this is so long…please help!

Bandil

  • Guest
Try this!
« Reply #1 on: July 29, 2004, 03:09:00 AM »
Sounds like your MDMA is quite pure. What temperature / pressure did it distill at?

Follow this writeup for the crystallization - very hard to fuck up:

Post 513755

(Bandil: "Easy preparation of HCl salt w/o gassing", Newbee Forum)


Regards
Bandil


endo1

  • Guest
DCM
« Reply #2 on: July 29, 2004, 12:03:00 PM »
I retried with DCM
MDMA-HCl is soluble in DCM dont use it here.

Does the ratio of solvent to freebase matter?
Yes, should be at least 4:1.

What temperature should the solvent/freebase be at and the HCI?
The colder the better, generally speaking.

If all or some of the freebase hasn’t changed from MD-P2P to MDMA will it still crystallize?
No, any mdp2p that didn't form the imine would be reduced to the alcohol.

Does the ph of the FB make a difference?
The PH of the fb/solvent should be about 7 when your done gassing.

What is over or under gassing?
When you gas too much or too little.

Is there any definite way of identifying is the freebase is MDMA?
Did you perform an a/b before distilling? If so then you probably have quite pure free base. If not then you may have some alcohol present interfering with crystalization.

Snakebyte

  • Guest
It sounds to swim that you might be ...
« Reply #3 on: July 29, 2004, 03:36:00 PM »
It sounds to swim that you might be overgassing.  Check your pH level with a wet strip.  When swim gasses there aren't huge clouds of puffy crystals belowing out.  Instead there is only a cloudy solution.  Then after swim puts the toluene in the freezer for awhile, the crystals will accumulate on the bottom and only then are quite apparent.


biffman

  • Guest
This brings back memories
« Reply #4 on: July 29, 2004, 04:33:00 PM »
After untold experience with other methods SWIM sticks with cheap and readily available acetone for gassing and crystallization.  As long as your freebase is well distilled, and it is done under a strong vacuum so the temp doesn't climb too high (temp of decomposition anyone?) gassing with HCL to freebase in COLD acetone (it heats up during gassing) works just fine.
   Tare (weigh) the receiving flask for your freebase distillation so that you know how much freebase you have produced.  That way, after you crystalize, dry and weigh the product, you know if you have converted all the base.
  Sometimes it will not all be crystalized but when you evaporate the solvent (which you should always save) any remaining product will often crystalize toward the end of the solvent removal.

biffman

  • Guest
Crystalizing...
« Reply #5 on: July 29, 2004, 04:42:00 PM »
As was mentioned  earlier by endo 1, you must be sure that you've done an a/b (acid/base) purification previously.
  But then again you should know that.

dave1234

  • Guest
Thanks for everyones help.
« Reply #6 on: August 01, 2004, 12:11:00 AM »
Thanks for everyones help.  How do you know if your overgassing?
I know had my freebase in way to much solvent...I can't wait to try again. 
I need to see white fluffy clouds...

jackhole

  • Guest
Gummy goo instead of powder.
« Reply #7 on: August 01, 2004, 12:36:00 PM »
You know you've been overgassing if...

the product forms into a gummy goo instead of powder.  :o


pooky

  • Guest
Gassing
« Reply #8 on: August 03, 2004, 12:37:00 PM »
P always uses acetone in a 3 to 1 (acetone/freebase)ratio with double distilled freebase.When you are gassing(using CaCL2 and HCL or Sulphuric)the mixture should be ice cold( just like biffman says).You will gas a  fair bit and it will start to get cloudy(this is when P does his little dance)then the snow storm begins.Gas until it warms up,dump in the freezer ( P has a pail of anti freeze at -20C to speed the process)and more crystals form.Don't gas under ph 7,when it gets to 7 put in the freezer again.
P suspects problems further back along the line...if you do have freebase and are gassing you will get snow.
Did you try the little crystals??


biffman

  • Guest
If an oil begins to form....
« Reply #9 on: August 03, 2004, 01:22:00 PM »
SWIM used to have that problem back in the early days but (as pooky mentioned) it seems to have been related to an incomplete or purification step earlier in the process. 
  As SWIM got better with his technique as time went by the "overgassing" problem disappeared.   Make sure that you have a strong enough vacuum for the distillation of the ketone so the temperature doesn't climb too high. 
  SWIM can gas as much as he wants but the product never reverts back to an oil anymore.
  Maybe SWIM just learned to do the magic crystallization secret dance a bit better.

dave1234

  • Guest
unstable isosafrole...?
« Reply #10 on: August 05, 2004, 11:05:00 PM »
Should my product crystalise in 500mls of solvent i.e xylene?  I have tried and tried with less but different batches.  I'm trying to work out where the problem lies. I did have some small ammount of crystals when I used acetone.  There thin, kind of transperent but like off white once placed altogether.  It's not the right product but seems like it's in the same ball park. 

I think maybe the problem lies back with the isosafrole that sat in acetone for a couple of months?? Is this possible?  Maybe the methlydioxy  (spelling) ring has been deranged...? It crystalised at MDP2P, producing a chicken fat like crystals..maybe their not correct...I did need to use bisulfate and some solvent for it to work. Does  anyone have any sugestions?  It looks like I'm back to the beginning...

indole_amine

  • Guest
acetone not suited for amine crystalization
« Reply #11 on: September 23, 2004, 08:38:00 PM »
Acetone is a ketone. Amphetamines are amines. Ketones and amines form imines under anhydrous conditions, giving off water.

Why do you all use acetone for making hydrochlorides??

Your amine will react with your solvent, and the water formed in this process will dissolve all salts you get from the remaining amine. Result: an equilibrium between dissolved amine*HCl and imine... :(

Suggestion: Use diethyl ether, EtOAc or other nonpolar solvent, and simply add enough dried, pre-gassed HCl/IPA (until pH 6.5), then add 2x the amount of cold, dry acetone and filter off. Voilà.

No need to bother with HCl gas, and you can even keep a small amount of your freebase amine, in case you add too much HCl/IPA: then you can simply revert the reaction by adding small amounts of the free amine, until pH is perfectly in the proper range, and proceed with acetone flooding.

Almost as easy as forming sulfates/phosphates...

indole_amine

pooky

  • Guest
???
« Reply #12 on: September 23, 2004, 10:43:00 PM »
Your amine will react with your solvent, and the water formed in this process will dissolve all salts you get from the remaining amine.

This makes P  wonder if  all that lovely powder that formed was a dream...or if all P's friends were lying when they told him it was the best they ever had.


indole_amine

  • Guest
Perhaps P first gassed a fb/nonpolar solution...
« Reply #13 on: September 26, 2004, 04:09:00 PM »
Perhaps P first gassed a fb/nonpolar solution and THEN added acetone? in acidic environment, imines don't form as readily.
But if P gassed a fb/acetone solution, I really wonder why it still worked.

Ah wait, I see: you gassed awhile before the salt suddenly appeared, right? This is because the pH first has to become acidic, then the imine is suddenly reconverted to the amine and acetone (reversible reaction), the amine readily reacts with the acidic solvent and lots of fluffy solids suddenly crash out of solution...

If you use a non-ketone solvent like IPA or toluene for gassing, you will only see a light cloudiness at first. You then add a bit acetone, chill in freezer for some hours (better overnight) and get beautiful crystals, not this white fluffy stuff. Because the crystals can form slowly, not suddenly and all at once.
Needs patience, but looks nicer.

(think about why you can form the imine between MDP2P and methylamine? Ketone and amine...)

indole_amine

pooky

  • Guest
Have..
« Reply #14 on: September 27, 2004, 04:54:00 PM »

indole_amine

  • Guest
of course not
« Reply #15 on: September 27, 2004, 05:11:00 PM »