Gassing the only way?

[PoohBear4Ever]

Regaring post-animation process of isosass:

Thought about the situation, and it would be nice to obtain honey in solid form without having to go outdoors to gas.  What would the downside be to adding dilute HCL(aq), and evaporating aqua?  Melting point of honey pretty low?

If washed with acetone, then re-xtalized, would purity be equivalent?

PB

[Rhodium]

Do it the Pihkal way, dissolve the freebase in twice the amount of IPA, add an equimolar amount of conc HCl, and then crash out all the HCl salt with a lot of diethyl ether.

If you recrystallize the MDMA*HCl properly, it will take care of any impurity included in the crystals by other inferior crystallization techniques (like simple evaporation).

[sunlight]

You can neutralize the base with aq. HCl, even with the solvent, then evaporate everything till 130-140 C (mp 147-151) and add 4 volumes of acetone to the brown syrup when it cools a while, with stiring, to see the deposition of crystals, filter and wash the cake with acetone. The product is what it has to be, but is a bit smelly and depending on the quality of ketone is snow white, white off or a bit tany. All the times I've checked the mp of this product was in the right range.
As Rhodium says is a inferior techinque, more a cooking procedure oriented to save solvents and get a product with enough, but not the best quality.

[Dope_Amine]

Disolve freebase in 3x volume of acetone, pipette in aq. HCl until pH ~4, throw in freezer overnight wake up with a smile.
something for your mind.......

[sunlight]

Dope, that sounds really good.

[Stanley]

What about the risk of formation of the imine? If it's a matter of a primary amine? E.g. amphetamine reacts with aceton in the presence of an acid (HCl) to form the N-isopropyl-amphetamine. Or with secondary amines the intermediate is formed, and is probably hard to recover. Or is this aspect negligible?

[Rhodium]

The isopropyl-substituted amine does not form unless a reducing agent is present, but I would worry about some imine formation using acetone as crystallization solvent. But if the "field testing" of this crystallization method works good for DopeAmine, then I guess that is just a theoretical worry.

[Acme]

Take the time to gas some MeOH with HCl to ~15-20% weight HCl.  Store this in the freezer, and use this soln for your acification needs.

[Dope_Amine]

What can I say.  I never thought about that and I never had to cuz it was never an issue.  I'm surprised that what I said was anything new around here.  I've mentioned this b4.  I wouldn't recommend acidifying past 2 although I've done that b4 too.  Anywayz, I've always done what I said above with good yield.  Back in tha day, I used to filter the crystals and then let the solution evaporate down to crystals and goo.  Then redisolve in a bit of acetone and throw back in the freezer for a second crop.  But now I wanna try Rhod's method cuz that sounds like fun!  So don't worry about it.  It works like a charm and is great for the lazy man.  It has always been my experience that when you evaporate down your mother liquor, there is always a bit of dark red/brown crap/oil inherent from the reduction.  Now if someone were to say that is the same color as imine, then I'd think maybee just a tiny bit gets converted to imine but still nothing worth fretting over.

BTW I accidentally made MDEA once while trying to methylate MDA cuz I used ethanol + acid + heat (<-not sure on the last one).  The GC/MS had mainly MDEA with a little bit of diethyl in there too!
something for your mind.......

[Jasium]

or you can just neutralize the freebase with conc hcl, and pour 4x ice cold acetone or ether on it and watch the instant xtal explosion. if you like to experiment you can form the sulphate by neutralizing with h2so4 in ipa 20% and  cold acetone. just remember the sulphate weights 20% more and if youre going to store it rextalise it.
j
"a peeping tom at the keyhole of eternity"

[Skindeep_Assrash]

Once you have your freebase in your non-polar (acetone is NOT a non polar) you can do Dope Amine's freezer route. it works like a charm. There's no need to get the free base in acetone though. Just make a teabag full of dried epsoms and dunk into freebase/non-polar for a good 30 min. This will dry the solution so when the HCl is added, one just shakes well and cools in the freezer for 10- 15 min.Crystal mass will form on the bottom of the flask. Or if you live in a cold area, just do the HCl dripping outside...It's snowing!  There's no need to GAS to reap  the salt. Just try and use the highest % HCl possible. if you get your HCl through a chem supply house it's usually the 8 stuff.


Don't forget to re-crystalize with cold dried acetone (dried if possible)

Sounds like fun.... sounds like something Assrash would like to see done for REAL. But this wont happen as Assrash doesn't break the law.

Assrash only predicts that these procedures will work fine.Damn fine.Awsomely. Perfectly!!!
-Assrash Ouch!

[Jasium]

if doing the hcl poured on the freebase route, use the 50% hcl from a chemhouse, if you can get it, then evap the acetone under a heat lamp to get what is trapped in the water, no gassing
j out
"fuck the media"

[LaBTop]

Totally BULLSHIT the last 3 posts!

And to the others:
Do you have only short memory?
We discussed this matter a long time ago several times, and the best solution ever found:

Use TOLUENE to mix with your DISTILLED freebase (3x more to 8x more) and neutralize with 33% HCl (=67% water in it!) or gas with 99% HCl GAS. An end pH of 4-3 doesn't hurt at all. You want to be sure that all freebase is converted to the chloride salt!

Then in case of the 33% HCl, boil off the water, filter crystals or just decant the toluene, in case of HCl gas just decant the Toluene (re-usable!), after all crystals precipitated,

then ALWAYS recrystalize your (wet or dried) IMPURE crystals by soluting in hot boiling ETHANOL or IPA (the minimum amount necessary to solute all crystals, these ALCOHOLS will keep all non crystallizable impurities soluted), and then add 3-4x icecold ACETONE (cold acetone also doesn't smell like hell!), let formed crystals precipitate, decant the alcohol/acetone off, wash crystals a few times with a bit fresh ACETONE, result: 99.9% pure endproduct.
(All extra HCl from the pH 4-3 overshooting when neutralizing your freebase will be soluted in your toluene, acetone, alcohol, so all these urban legends about burned lips and tongues, forget it!)

I'm not even going to look up the threads, should be common knowledge by now.
1. Use HCl gas (faster, cleaner)
2. If you can't get HCl gas , use 33% HCl. (In fact much safer from an acquisition viewpoint!) 

Big ADVANTAGE: TOLUENE doesn't smell 1 km around your "secret" lab! LT/  

PS: all these short step brainiacs drive me crazy, these are all wellknown labprocedures, any shortcut taken takes you a long way off from what is really possible in terms of purity and REAL yields.

Especially the idiots who tell me: but then I loose precious WEIGHT !
I hope you loose so much weight yourself that it becomes inpossible to multiply or set one step in a lab, stupid fuckers! LT/  
WISDOMwillWIN

[RoundBottom]

please LT, don't hold back, tell us how you really feel.  

is it necessary to watch the pH while gassing? 

also, SWIM has seen bad things while trying to gas all the salt out at once.  SWIM ends up gassing the same toluene many times, a la dr gonzo's photo essay; up to 7 times on a 2x MM Nitro Al/Hg. 

if SWIM tries gassing it all out at once, the salts get very dirty, a medium yellow or brownish colour.  why is this?

[Rhodium]

You cannot check the pH of a non-polar solution. A good way is to have a damp pH paper above the solution being bubbled, when HCl gas escapes the solution without being absorbed by the solution, you're done.

[Jackhammer]

Good point Rhod...SWIM had some isopropyl substituted MDA lately....could not figure out where it came from but your remark makes sense. BTW imine formation is observed by SWIM but only to a very minor extent.
I'm more curious about the things I dream than about things I see when awake!

[Dope_Amine]

You can check the pH of acetone by wetting a pH paper, shaking the excess water off and dipping. 

If you crystallize reasonably clean product from acetone or you gas DCM (for MDA) you DO NOT have to recrystallize. And my standard of purity is only the whitest of white.  C'mon LaBTop, and boiling off water from toluene sounds like a bitch.  Any of these methods if done right will produce extremely pure white crystals.  For MDA, gassing in DCM is of course the prettiest with the big fish scales.  But I believe the 2nd best method for MDA and THE BEST method for MDMA is to simply add aq. HCl to product in acetone.  As far as ease of set-up and execution, I don't think anything is as easy as acetone + aq. HCl.  The new improved version below was tried after the discussion of imine formation and differs from old in the temp of addition and the concentration of amine.


Light golden MDMA freebase was disolved in ~6x it's volume of acetone.  It was found that making the solution more dilute than the old 1:4 was very benificial because crystallizion can occur without any cooling.  The flask was placed in an icebath on top of a stirrer and the solution was allowed to rapidly stir and cool down.  Next, conc. aq. HCl was slowly pippetted (really fast dripping) in repeatedly and the pH was checked with water wetted pH strips until the pH was 2-4.  About a third of the way through the addition of HCl, the solution will have exploded with granular crystals (like NaCl as opposed to fishscales from DCM crystallization).  The flask is covered and placed in the freezer overnight and the next morning, the solution is filtered to recover ~90-96% of the product.  If the product oil was dirty then washing with a bit of ice cold acetone will clean and lighten it up.  Evaporate down the mother liquor, redisolve in 1/3 the original amount of acetone and throw back in the freezer to recover the final bit of product.  


something for your mind.......

[PoohBear4Ever]

kapten, 

I understand that gassing is far less difficult than the synthesis itself; however, I would prefer to dream everything inside, never leaving untill glass is clean, and product is in hand.  If SWIP uses a gassing setup, he plans on using his filter flask, with a seperatory funnel on top.


But let's not start counting chickens before the eggs hatch,

PB

[foxy2]

You could gas with one of the set-ups that some use.  They pump air(aquarium pump) thru conc. HCl to carry residual HCl gas via tube to gas product.  Way slower but much safer, very controllable, definately need a drying tube though.
Do Your Part To Win The War

[PoohBear4Ever]

How slow are we talking about?  Also, couldn't one gas indoors using a bong-like apparatus, where extra gasses are passed through to a hose going outside, or to a closed system aspirator station?

PB