Author Topic: Alternative To Gassing Ideas?  (Read 6865 times)

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Bubbleplate

  • Guest
Alternative To Gassing Ideas?
« on: October 07, 2002, 06:23:00 PM »
After SWIM experienced the joys (NOT!) of gassing, you know the wonderful clouds of HCl wafting thru the summer air, he is determined to find a "kinder gentler" route to end product.
After looking through the FSE, have come up with the following and would like opinions, other ideas:
Post MM Al/Hg: Combine A/B with Titration
1) Extract Xylene with 2x 100 ml 10%HCl.
2) Basify with 30% NaOH.
3) Extract with 150 ml Xylene.
4) Extract Xylene with 100 ml 10% HCl.
5) Evaporate H2O.
6) Recrystalize from dry IPA.
Comments? Suggestions?

If they drive God from the earth, we shall shelter Him underground - Dostoevsky

Diggity

  • Guest
What was your problem with gassing???
« Reply #1 on: October 07, 2002, 06:52:00 PM »
What was your problem with gassing??? Swim loves gassing. He even has a little dance he does right before he collects his crystals. What was the problem?? Im sure if you did it right, you too would be happy.

& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

goiterjoe

  • Guest
modifications
« Reply #2 on: October 07, 2002, 06:54:00 PM »
extract with toluene/xylene as usual, acidify with hydrochloric acid, basify and extract with DCM, strip off DCM, fractionally distill, take up in IPA, neutralize with concentrated HCl, crash out with ether, filter, wash with ether.

All paths are the same: they lead nowhere

El_Zorro

  • Guest
or..
« Reply #3 on: October 07, 2002, 06:59:00 PM »
Maybe extract with HCl(aq), basify, extract with NP, vac distill FB, dissolve FB in IPA, titrate with HCl(aq), vac distill off a large portion of IPA/H20, dump in 2-3x volume of acetone, freeze, dump in buchner.  Vac distill off more IPA/H20 from filtrate, dump in more acetone, if any more crystals, dump in buchner.

Who is that masked man?

Bubbleplate

  • Guest
Gassing May Be Fun For Saddam
« Reply #4 on: October 07, 2002, 07:29:00 PM »
But not for me! You can't do it indoors; No matter how careful/slow you do it, some residual HCl gas is wafting around, dissolving the finish on my hotplate and my lungs. And you're left with a nasty acidic salty mess to clean! And that Sulfur smell - hmmmmmm. Just keeps on going and going....

If they drive God from the earth, we shall shelter Him underground - Dostoevsky

Rhodium

  • Guest
You've made 1.25 gram MDMA crystals?
« Reply #5 on: October 07, 2002, 07:42:00 PM »
You've made 1.25 gram MDMA crystals? What was the crystal shape?

wyndowlicker

  • Guest
Send one this way.
« Reply #6 on: October 07, 2002, 07:52:00 PM »
hell yeah diggity!You do that dance too!And Max send a double terminated crystal this way.Need it for a crystal healing configuration. :P

You can tell the queen of diamonds,by the way that she shines.-GD

goiterjoe

  • Guest
somewhat cubical
« Reply #7 on: October 07, 2002, 08:04:00 PM »
I've had one gram crystals form before, and they were rectangular in shape, clear, and beautiful to look at.  It almost made me cry to have to take a razorblade to them.

All paths are the same: they lead nowhere

pickler

  • Guest
A very simply way to get your crystals is as ...
« Reply #8 on: October 07, 2002, 08:38:00 PM »
A very simply way to get your crystals is as follows. Work up your MM al/hg as usual. Do all of your washes on your tol or xylene. Make  5-10% acidic water. Put your xylene/toulene in a sep funnel and add your acidic water. You can watch the mdma freebase migrate to the water layer. Shake a few times and let seperate. Tap off water layer and evap till you get a syrup. Let cool and add a bit of acetone. Crystals everywhere. Clean as usual. Don't thank me, thank noj.

I went into the business for the money, and the art grew out of it.-Charlie Chaplin


Neron

  • Guest
Up close... real close...
« Reply #9 on: October 07, 2002, 11:14:00 PM »

http://146.201.224.61/pharmaceuticals/pages/mdma.html




MDMA under a scanning-electron microscope.

Tis' an ill wind which blows no minds
 - Discordia

Mountain_Girl

  • Guest
Look at the colors man
« Reply #10 on: October 08, 2002, 12:50:00 AM »
Gosh, and they said MDMA is not a psychedelic...
:P

Mountain Boy

hest

  • Guest
gassing
« Reply #11 on: October 08, 2002, 01:12:00 AM »
Bubbleplate, back to the subject. Iff you make a solution of HCl in ether or alcohol you just drip this solution into your dry toluen/frebase until your wet pH paper shows that the solution is acid. Can't bee easyer than that.
Making the stock solution is a one time job.

Bubbleplate

  • Guest
Thanks All For Your Help
« Reply #12 on: October 08, 2002, 05:50:00 AM »
BTW, SWIM got 14g honey on first try - probably due to weak nitro. Feels good to have gone the whole route. Now can improve technique.

If they drive God from the earth, we shall shelter Him underground - Dostoevsky

Rhodium

  • Guest
Single-crystal MDMA.HCl as distribution form?
« Reply #13 on: October 08, 2002, 08:28:00 AM »
Would it be possible to grow several uniform crystals? Wouldn't it be a very cool to grow crystals, aiming for a weight of 120-130mg, and then use single-crystal MDMA.HCl as distribution form? That would be way better than pills or capsules not only from an aesthetic point of view - who could cut or otherwise tamper with a uniform crystal? A clear rectangular crystal of MDMA.HCl always has the same size, so people would know how big it would suppose to be... Any takers?

TheBlindGenius

  • Guest
Stock solution
« Reply #14 on: October 08, 2002, 09:00:00 AM »
Hest, would you have to gas to get that stock solution?  Could there be a way of doing it by first mixing regular 37% HCl w/ alcohol or ether then removing the water chemically, for example using CaO or anhydrous something or other?

Bubbleplate

  • Guest
Crystals: Couldn't You Do It Like
« Reply #15 on: October 08, 2002, 09:02:00 AM »
growing "Rock Candy"? i.e. make a supersaturated solution and put in a chamber that had weighted cotton threads suspended in it. Simple. Maybe even roll the wetted threads in some fine powdered material first to have some starting points for the crystals.
Granted the crystals wouldn't all be the same size, but tweaking the solution strength you might get fairly consistent sizes.  When done, cut off the individual crystals.

If they drive God from the earth, we shall shelter Him underground - Dostoevsky

Rhodium

  • Guest
Homegrowing
« Reply #16 on: October 08, 2002, 09:26:00 AM »
Madmax: I don't have any links up my sleeve at the moment, but there are loads of crystal growin sites available on the net.

Genius: Acros and others sells 5 M HCl in IPA very cheap.

TheBlindGenius

  • Guest
Stock solutions
« Reply #17 on: October 08, 2002, 09:39:00 AM »
Rhodium-- I know, however, it would be much better if it could be made at home, especially since I do not have an account with Acros or any of the big domestic chemical companies.  I only have access to smaller chemical companies that do not carry HCl/IPA or HCl/MeOH, etc, and also access to some overseas chemical companies, and shipping corrosives internationally is expensive.  It would be nice to know how Acros, etc. make their stock solutions.  Do you think the method I described would work at all with any "water-removing" chemical?  I am very interested in this topic because I hate gassing and have burned my lungs numerous times and also my skin even with gloves on.  Not only clandestine, but in the academic lab.

Barium

  • Guest
How is the 5-6 N HCl/IPA from acros made?
« Reply #18 on: October 08, 2002, 09:49:00 AM »
How is the 5-6 N HCl/IPA from acros made? By gassing!!
Adding CaO to wet HCl in IPA would be a good, but expensive, way to get CaCl2.
Why don´t you simply follow more experienced bees advice and devote one, just one, day to make your stock solution of HCl in whatever-solvent?

Catalytic hydrogenation freak

pHarmacist

  • Guest
salt
« Reply #19 on: October 08, 2002, 09:55:00 AM »
Well, HCl salt is an option, but surtenly not when it comes to amphetamine (european bees know what I'm talking about). Why? Becouse amphetamine.HCl is highly hydroscopic and the street name for the amph.HCl overhere is "goo-speed"... Anyways, phosphate salt is to prefer, this is a piece of information taken from rhodium.ws that can bee useful:

"....135 g (1 mol) of amphetamine freebase were stirred into 300ml of acetone in a 1000ml erlenmeyer flask. To the resultant solution there were slowly added under constant agitation 115.3 g of 85% phosphoric acid (containing 1 mol of H3PO4), care being taken to avoid any sudden rise in temperature or local overheating due to the considerable amount of heat that is evolved. During the addition of the phosphoric acid a fine, white, flocculent precipitate appears which becomes more and more dense and abundant, as the quantity of added acid increases.

When the entire quantity of the phosphoric acid has thus been added, agitation of the mixture is continued for about a half-hour or more to insure complete conversion. The precipitate is then allowed to settle, the supernatant liquid is drawn off, and the residue is filtered. The precipitate thus separated is washed with acetone and is then dried by evaporation to constant weight. It forms a fine, white, impalpable powder consisting of pure monobasic amphetamine phosphate.

Reference: Pharmaceutical Manufaturing encyclopedia (1988)..."

[pH]armacist - Never underestimate the power of retrosynthesis. Svenskar suger på fotboll!