Author Topic: Citric acid direct to freebase  (Read 362 times)

Bardo

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Citric acid direct to freebase
« on: May 01, 2011, 11:58:54 PM »
Ok after making the hcl mda salt many times I wanted to switch things up strictly for the reason of saving time. Usually I'll take a xylene solution with mda freebase in it (that did not go through an A/B extraction because I've found it unnecessary) and add %5 hcl then extract out the water layer to evap. I've gotten sick of this method because I have to sit around for freakin ever to wait for %95 water to evap away and I can't use stronger hcl or else there are tarring problems. So in order to cut down on that evap time I was thinking of switching to citric acid dissolved in %95 ethanol. Then I figured screw it water is always a problem when salting mda so lets get rid of that %5 water and just go with denatured alcohol which is %50 ethanol %50 methanol (not worried about the methanol since it will after all completely evap). But then I was thinking, wait a second, alcohol evaps very quickly but citric acid is a solid so does it even need to be in a solution first anyways??? So can I just drop solid citric acid crystals directly into a xylene/freebase solution and expect to just extract out the mda citric salt easily? I have been told salting with citric acid can lead to a goo but this was from someone who had water in his system and from my experience water really causes the gooing/tarring/crapping up problems with mda salting. What do you think?

jon

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Re: Citric acid direct to freebase
« Reply #1 on: May 02, 2011, 01:55:44 AM »
alcohol/ether or petro ether it's called dual solvent recrystallization

Shake

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Re: Citric acid direct to freebase
« Reply #2 on: May 02, 2011, 02:33:14 AM »
citrate crystals tend to go from hard goo to shiny xtals by rinsing them with warm naptha.. an easy way is extracting the xtals with filtered lemon or orange juice then evap and naptha wash

im with you though i hate waiting for water to evaporate. so can you acidify the xylene directly? it would have to be dry for xtals to just fall out.. jon uses a different method, where his freebase is in DCM so its easy to strip off down to the freebase, where he then titrates the mdma oil with .5 molar qty of citric acid then just pour in 2 different solvents at a ratio of 1:5 ethanol to petro ether or naptha, then chuck in freezer for a couple days and wait for xtals to form.. the resulting half formed xtals might be gooey, should dry in the oven.

as for what to do when you have a litre of xylene and your supposed to strip it all off or evap it, you are sorta up shit creek unless you want to muck around distilling again, but usually by this time you want to just get it over with



« Last Edit: May 02, 2011, 02:48:42 AM by Shake »

jon

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Re: Citric acid direct to freebase
« Reply #3 on: May 02, 2011, 02:42:48 AM »
1:5 is close better 1:3 also the mdma oil should be striped of water by heating under a vacum, so you get definite crystals.
otherwise you get this amorphous goop which is fine if you just want to get high.
the average custie does'nt like it.
they think it should come on hard in 15 minutes i get calls about that stark raving mad people thinking they gettin ripped in my voicemail but the funny thing is toward the end of the message you could hear thier voice soften a little as it's kicking in.
i never returned those calls and never talked to those people again, fuck them.

Bardo

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Re: Citric acid direct to freebase
« Reply #4 on: May 02, 2011, 05:08:33 AM »
Distilling? I don't mess around with that time consuming stuff. If I can bypass an A/B because I don't find it absolutely necessary I can do without other things as well (think more commercial and less connoisseur).  

Look if I got a few liters of highly yummy xylene in a sep funnel (I got some big sep funnels) and I toss in and shake around some citric acid should it stay in the xylene or drop out? If it stays in xylene then if I added the citiric dissolved in alcohol instead then shouldn't that give me a layer to extract out so that I could just then evap to recover the goods? I don't even care if it's goo. Any goo or tar can be put in a food dehydrator, turned brittle, and then chopped up into powder in a food chopper/processor (but if I'm using denatured alcohol there will be no water present). You guys are thinking what makes the purest, cleanest, prettiest stuff and I'm thinking what makes passable stuff the quickest. Ethanol/methanol evaps so quickly I probably don't even really care if I have to use it in order to make an extractable layer for the mda citrate to go into. I just want to know if in theory there shouldn't be any issues. Again my main issue is getting around waiting for freakin ever for %95 water to evap when making the hcl (no lets not bring up gassing).
« Last Edit: May 02, 2011, 05:10:57 AM by Bardo »

fractal

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Re: Citric acid direct to freebase
« Reply #5 on: May 02, 2011, 05:30:09 AM »
Distilling? I don't mess around with that time consuming stuff. If I can bypass an A/B because I don't find it absolutely necessary I can do without other things as well (think more commercial and less connoisseur).

That's really messed up. The fact that you plan on selling it should be reason to make it as clean as possible. Your not only messing with your health.

Shake

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Re: Citric acid direct to freebase
« Reply #6 on: May 02, 2011, 08:12:30 AM »
Quote
Usually I'll take a xylene solution with mda freebase in it (that did not go through an A/B extraction because I've found it unnecessary) and add %5 hcl then extract out the water layer to evap.

are you saying you dont even water wash or brine wash before you extract your crystals?

I hope you at least do that!
« Last Edit: May 02, 2011, 02:19:56 PM by Shake »

Bardo

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Re: Citric acid direct to freebase
« Reply #7 on: May 02, 2011, 03:15:30 PM »
Distilling? I don't mess around with that time consuming stuff. If I can bypass an A/B because I don't find it absolutely necessary I can do without other things as well (think more commercial and less connoisseur).

That's really messed up. The fact that you plan on selling it should be reason to make it as clean as possible. Your not only messing with your health.

Who ever said anything about selling? And my stuff has been tested at %99.9 purity by state labs.... And where in the hell is distilling required???? Why the fuck would anyone go through the time consuming process of distilling a temperature sensitive freebase from a perfectly good and clean nonpolar extract??? Who distills their freebase from their solvent instead of just gas out or salt out directly from the solvent??? You guys are strange.

Shake

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Re: Citric acid direct to freebase
« Reply #8 on: May 02, 2011, 03:34:38 PM »
calm the fuck down, did you wash the hg salts out of your xylene extracts?

mdma freebase can (but certainly does not have to be) distilled under vacuum no problem same as your ketone should have been, as it mostly likely will double your yeilds, what synth are you using? clearly you are not distilling anything here but hey, if thats how you do it so be it i dont care.

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Who ever said anything about selling?

you did

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I can do without other things as well (think more commercial and less connoisseur). 

thats what commercial means brother.

all that matters is that you dont skip vital washes after you extract your freebase into your solvent.

as for your citrate question, it is a good question, i dont know the answer but i def want to. when you find out let us know.. jon is the only citrate guy we have here and he doesnt like going into specifics much
« Last Edit: May 02, 2011, 03:39:25 PM by Shake »

poisoninthestain

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Re: Citric acid direct to freebase
« Reply #9 on: May 02, 2011, 07:12:58 PM »
For MDA.citrate crystallization pull free base amine with nonpolar solvent, brine wash it to get rid of the polar junk, and titrate in .5 mol eq citric acid or hydrate in a minimum amount of water or EtOH...in all the times I've performed this with citric acid I was never greeted with nasty tar(H2SO4 and HCl are a different story)...this can be quickly evaped on a stove, hotplate, or a propane flame...once the solvent volume becomes reduced down to the last cc's you'll see a thick paste-like goo...once this happens add a little more heat until it gets thicker and thicker until it's almost semi-solid...kill the heat and stir it a bit as it cools down...it should form pinkish-red(most of the time depending on the previous reaction you used to arrive at the amine)crystals.  Recrystallization with an ethanol:xylene system gives off rhombus crystals that are beautifully bitter.

Also if one is lazy you can dump your amine citrate solution or impure crystals(never tried actual "goop" as someone put it) into an excess anhydrous IPA solution saturated with citric acid...the amine citrate will precipitate out almost immediately and even more with freezing as white crystals...the solution itself will remain a blood red if your impure starting product was pink-red...all this is due to the common-ion effect...haven't tested it on MDMA.citrate as of yet.

Bardo

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Re: Citric acid direct to freebase
« Reply #10 on: May 03, 2011, 02:29:07 AM »
Also if one is lazy....

Thank you! Finally someone was understanding what I was getting at! Thanks poison, I think I got it now. In the end it seems I should expect a goo (verses a tar hcl style) but that is something I think I can deal with with just a food dehydrator. In the end a very quick evap to a goo put in a food dehydrator should be much quicker then waiting for freakin ever for %5 hcl to evap (granted no goo or tar though).


...And Shake I said THINK more commercial in order to understand the time saving I'm trying to get at, I did NOT say "hey I'm sitting over here making kg batches of schedule 1 for sale".

jon

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Re: Citric acid direct to freebase
« Reply #11 on: May 04, 2011, 10:41:11 PM »
nice to see youse guys digging that citrate.
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Who ever said anything about selling? And my stuff has been tested at %99.9 purity by state labs

bardo what kind of 'state lab'?
the only ones i know of are crime labs you know forensic labs, what did you do mail some in to your local forensic lab?
strange they offer this service?
« Last Edit: May 04, 2011, 10:48:07 PM by jon »

psychexplorer

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Re: Citric acid direct to freebase
« Reply #12 on: May 05, 2011, 03:19:08 AM »
I'd like to know that too.

The DEA prohibits anyone with a schedule I license from assaying purity or active weight. This is why DanceSafe's testing lab can only give a yes/no on the compounds in the samples sent in for testing.

The DEA went out of their way to write the rules to prevent licensed labs from becoming QC for manufacturing ops.

hypnos

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Re: Citric acid direct to freebase
« Reply #13 on: May 05, 2011, 04:05:09 AM »
   Well spotted jon,  I read that too, but being where I am and all, didnt pay much

 mind...we're a tad more relaxed...hmmmm.......typo possibly................................?
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Shake

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Re: Citric acid direct to freebase
« Reply #14 on: May 06, 2011, 11:39:41 AM »
in order to prevent mis information being spread, i would like to say that lemon juice from a squeezy bottle from the store does not work and will turn your crystals to a gunk due to all the additives they must put in it. embarresing. BUT i have gotten nice crystals from squeezing a fresh lemon into water and extracting that by evaporating on a big plate.

problably just get the citric acid powder though. the only reason lemon juice looked good to me is because the ph is already 4-5 so you dont over shoot easily like hcl

Shake

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Re: Citric acid direct to freebase
« Reply #15 on: May 06, 2011, 11:55:02 AM »
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And my stuff has been tested at %99.9 purity by state labs


haha funny, some of the solvents you are using to finish your stuff up with probably are not even that pure.. are using xylene not toluene means you are getting it from a hardware. and probably even the one near me becasue the xylene on the shelf is always empty! why would you go making that up? pfff 99.9 my ass

also, i know chemists who distill thier sass to safrole, distill thier ketone, then distill thier mdma across aswell then work with that clear mdma oil.. that is 99% material, not your shake and bake stuff
« Last Edit: May 06, 2011, 12:22:05 PM by Shake »

micro

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Re: Citric acid direct to freebase
« Reply #16 on: May 30, 2011, 10:21:57 PM »
Citric acid is not apparently as availabe out there as it is here.
As I'd suspect that people would not extract it from lemons for just the fun of it.
Just to tease, it is available otc and is from 3 to 9eur for 100g.

fractal

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Re: Citric acid direct to freebase
« Reply #17 on: May 30, 2011, 10:59:22 PM »
Citric acid is available otc everywhere.

hypnos

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Re: Citric acid direct to freebase
« Reply #18 on: May 31, 2011, 02:02:24 PM »
 Sure is! Try ANY supermarket!
"the two things you can give away and never lose, are what you know, and how you feel...."

Methansaeuretierchen

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Re: Citric acid direct to freebase
« Reply #19 on: June 02, 2011, 02:03:48 AM »
Fast way from amine to salt I used several times:
Make dry HCl gas by heating NaHSO4 (Pool PH minus) and NaCl on a hotplate etc..
Bubble the gas through IPA until it's saturated. (You can store this solution!)

Dissolve base in DCM (dry with waterfree NaSO4 if neccesarry) and add IPA/HCl solution until it's acidic.
Evaporate DCM and bingo.