Author Topic: Largescale DMT alcohol cake extraction method?  (Read 552 times)

overunity33

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Largescale DMT alcohol cake extraction method?
« on: October 05, 2010, 09:14:51 PM »
Anyone who has done STB at the kg+ level knows its a touchy bitch and a lot of work.  I found this tek here:
http://www.entheogen.com/forum/showthread.php?t=25915

If you guys give me some good advice I will have my friends try it at the 5kg level and post results.

I have a few questions:
1) it says to add the base to the alcohol, I assume you add equimolar base or slightly more compared to the amount of dmt you expect to extract in order to freebase the naturally occurring salts, so 1kg should require less then 100g of base, which is nice compared to the 500+g you need for a STB.
2) some people speculate that using MeOH and NaOH you may generate sodium methoxide, which would degrade your spice, is this true? I would rather not have to worry about keeping my meoh anhydrous.  I guess an easy workaround would be to use KOH.
3) Would you have to evaporate most of the MeOH before pulling with naptha or can you leave some?  Do you have to evaporate at all after steeping and filtering?  I guess my real question is: are naptha and meoh miscible?

Let me know, thanks.

Vesp

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Re: Largescale DMT alcohol cake extraction method?
« Reply #1 on: October 06, 2010, 12:16:19 AM »
KOH would be so much worse than using NaOH.
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Sedit

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Re: Largescale DMT alcohol cake extraction method?
« Reply #2 on: October 06, 2010, 12:23:11 AM »
Having sadly never gotten to extract DMT due to inability to possitively identify the correct species I have envisioned it for many years now and think that this theoretical would work pretty well.

Alcohol or Acetone extraction simular to the procedure in discussion allowing a slightly basic PH at the verylest thru the use of NaOH to ensure your target comes along.
Evaporate slowly to dryness since to high heat and the already high PH could damage to many things creating variables such as Saponification of any fats creating a world of hurt later on down the road.

Once dry lower the PH with Either HCl of Acetic acid I guess would work and once again evaporate to dryness this time grinding your cake as much as possible.
A solvent boil which has not been decided upon but something to remove all or most nonpolar, non alkaloid componds. Multiple nonpolar solvents would be the best possible option assuming you are able to dry them enough to ensure nothing is lost.

At this point you have your options of cold precipitation or quite possible gassing to obtain the HCl salt which you can dry and base to make sure you have pure DMT in the nonpolar you freeze out.


This should in theory work pretty well for DMT since its effective in many alkaloid extractions.


[edit]


Yup forgot to mention that, KOH is a stronger base then NaOH meaning that the equilibrium will lay further to the right which is not what you seek in this case.
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overunity33

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Re: Largescale DMT alcohol cake extraction method?
« Reply #3 on: October 06, 2010, 04:30:04 AM »
Thanks for the advice.  My plan would be to heat 60C with meoh + base, filter the material and then evaporate the methanol down.  Once it is dry (or maybe just boiled down some) add a little bit of heavily basified water and then extract with hot naptha until the naptha comes off clear.  Freeze crystallize this and there you go. 


overunity33

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Re: Largescale DMT alcohol cake extraction method?
« Reply #4 on: October 22, 2010, 05:48:55 AM »
So my friend took my idea and ran with it.  He heated 2kg very finely powdered mexi mh rootbark covered with about 3L of methanol/100g NaOH at 40c for 3 hours.  Well he tried to filter it afterwards and realized that only about 10% of the solution was recoverable even with compression due to the slurry from the very fine powdered rootbark.  He added the 10% back to the rootbark and let it sit for a week or so before he mutilized an ac unit so he could perform vacuum filtration on this scale.  Well this slurry was so thick it worked even less then 10%.  He plans on evaporating the methanol from this material and using familiar methods to extract.  Moral of the story is if you try this method do not use fine powdered rootbark, use the shredded stuff.


I told my friend the speculation of freebase degrading in those conditions and it might not be worth his time removing the methanol and doing a standard "STB".  Do you guys think my friend is screwed?  Seems to me dmt freebase could survive those conditions, but I also noticed sodium methoxide could be formed which is a very strong base and could harm the freebase after a week of storage?

micro

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Re: Largescale DMT alcohol cake extraction method?
« Reply #5 on: October 28, 2010, 07:00:13 PM »
Well damn, some 1,5kg of concentrated powdered innerrootbark powder was acquired.
A "small" scale version of the cake method was tried, with the cake just now waiting to be extracted.
200g of powdered bark. Due to the bark being a fine powde,r filtartion pretty much impossible, only something like 100ml to 200ml max of the 600ml of Caustic denat.EtOH used was recovered in filtration.
The cake will be extracted with toluene and possibly xylene.
This should produce a "full spectrum extract" with all three alkaloids (NN-DMT, yohombine and the mystery six precenter). The extract will then be extracted with high quality "purified gasoline" (~6e/100ml at the pharmacy, very pure and good for extractions, also the only good source) to separate nn-dmt from the other two. The n-oxide of dmt will mostlikely be present due to the failed filtration and thus exposure to air.

I'm just so glad that there is a thread on this here just when it is most interesting.

overunity33

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Re: Largescale DMT alcohol cake extraction method?
« Reply #6 on: October 28, 2010, 08:57:44 PM »
Yeah this cake method should only be done with shredded bark thats like pencil shavings.

micro

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Re: Largescale DMT alcohol cake extraction method?
« Reply #7 on: October 29, 2010, 03:38:47 PM »
Yep. so it seems. The ~100ml of filtered EtOH gets evaporated and extracted.
The rest of the cake gets itself based and extracted with xylene.

delafonze19

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Re: Largescale DMT alcohol cake extraction method?
« Reply #8 on: July 06, 2011, 10:21:33 PM »
So this guy I know threw 5kg in a 5 gallon bucket. Impossible to work with. Set it aside in storage unit for a month or two. Pulling tons of n-oxide now that he has time to work with it. He has no zinc powder handy, but heard aluminum may be more effective for reducing anyway. The question is must it be aluminum powder or would some soda cans be good enough? Lame first post, I know, but that's the way it goes sometimes

antibody2

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Re: Largescale DMT alcohol cake extraction method?
« Reply #9 on: July 11, 2011, 11:31:05 PM »
1) it says to add the base to the alcohol, I assume you add equimolar base or slightly more compared to the amount of dmt you expect to extract in order to freebase the naturally occurring salts, so 1kg should require less then 100g of base, which is nice compared to the 500+g you need for a STB.

A better plan would be to get a hold of ph test strips and add base until you are at the correct ph. After you do the 1st extraction check the ph again, you may need to add more.

2) some people speculate that using MeOH and NaOH you may generate sodium methoxide, which would degrade your spice, is this true? I would rather not have to worry about keeping my meoh anhydrous.  I guess an easy workaround would be to use KOH.

That isn't going to happen, we've been adding NaOH to post MeOH Al/Hg rxns for decades with no problem.

Would you have to evaporate most of the MeOH before pulling with naptha or can you leave some?  Do you have to evaporate at all after steeping and filtering?  I guess my real question is: are naptha and meoh miscible?

I would reduce the MeOH volume for the simple reason that it is easier to extract a smaller volume than a larger volume. To answer your question though, Naptha and MeOH are not miscible, but they will mix to some extent. What will happen when you add your aqueous base is the MeOH will migrate to the aqueous layer as MeOH IS miscible with water, even water that is saturated with salts.

If you would like some unsolicited advise, I would remove all the MeOH from your cake, dissolve the residue in a dilute acid HCl or Acetic, filter to remove solids (tannins etc), slowly basify with aqueous NaOH then extract that with naptha. You will end up with a purer product that way. This way you can also use a sep funnel. Basifiing directly the cake and extracting the resulting soup will have solids that will clog your sep funnel.

Vesp

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Re: Largescale DMT alcohol cake extraction method?
« Reply #10 on: July 12, 2011, 08:00:27 AM »
You might need to be careful about aldehyde formation, however as it will react (possibly) and form beta-carbolines which are not easily extracted via A/B techniques and this could lower your total alkaloid extraction yeilds...
Perhaps NaOH + other present organic substances => aldehydes? highly unlikely...
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shroomedalice

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Re: Largescale DMT alcohol cake extraction method?
« Reply #11 on: July 12, 2011, 09:54:12 AM »
whats wrong with straight alcohol ?

antibody2

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Re: Largescale DMT alcohol cake extraction method?
« Reply #12 on: July 12, 2011, 02:03:05 PM »
whats wrong with straight alcohol ?


Nothing wrong with it. It will work for this tek. But in many parts of the world MeOH is available in hardware store at $10/4l whereas 95% EtOH tends to be more expensive and/or difficult to acquire. Like in Canada, where 95%+ EtOH is only available from a chem suppliers. MeOH also has a lower BP, which makes its removal easier.

The Lone Stranger

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Re: Largescale DMT alcohol cake extraction method?
« Reply #13 on: July 12, 2011, 03:37:31 PM »
"whats wrong with straight alcohol ?"

Exactly . Same with pure aceton . Or what is jungle spice made with ? Its a red waxy extract that is said by many to be better than pure DMT .

Another thing is fuck chemicals ..... what about pure water , then filtering and then drying ? I`ve seen and had ayahuasca that had been filtered and thickened and it was REALY good . It looked like and had the consistency of good sherry . If the water had been evaporated the goo would have been very good .

On DMT-nexus the "experts" moaned at me for asking about useing KOH and said it can produce some nasty side products when used to extract DMT ?

As to "meths" = methylated spirits one has top be carefull if one doesnt live in europe . Here they are not allowed to make / sell maths that has anything in it in any quantity that can harm a person . Its made from 94 % ethyl alcohol plus some aditives like MEK , benzin and Pyridine to make it taste shitty .

Someone i know uses it for extractions . The extract gets filtered and then heated so the alcohol evaporates . Then when it starts to get greasy he throws water in to it = the shit mixes with the water and the oily extract goes hard = he can then just throw the watery / greasy goo away and ends up with a product that tastes good and doesnt do anything nasty .

Harmala alkaloids from P:Harmala can be extracted with water .

Comments / advice please ?
« Last Edit: July 12, 2011, 03:43:53 PM by The Lone Stranger »

antibody2

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Re: Largescale DMT alcohol cake extraction method?
« Reply #14 on: July 12, 2011, 06:35:09 PM »
On DMT-nexus the "experts" moaned at me for asking about useing KOH and said it can produce some nasty side products when used to extract DMT ?

Harmala alkaloids from P:Harmala can be extracted with water .

Comments / advice please ?

The DMT Nexus is a great place with lots and lots of great info. But chemistry is not their long suit (with the exception of a very few members), so take it with a grain of salt. There is a lot of superstition being passed off as science.

Harmlas can be extracted with water and a small amount of vinaegar. You might get away with just water as the harmlas are already in salt form, but a little vinaegar is a cheap insurance policy.

Jungle spice is dmt that has been extracted with a less selective solvent than naptha, such as toluene, xylene, ether or DCM, it pulls all kinds of other stuff out of MHRB, which is why it isn't white, it isn't remotely pure. Here is a paper on the subject if you are interested.

delafonze19

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Re: Largescale DMT alcohol cake extraction method?
« Reply #15 on: July 12, 2011, 06:45:44 PM »
So this guy I know threw 5kg in a 5 gallon bucket. Impossible to work with. Set it aside in storage unit for a month or two. Pulling tons of n-oxide now that he has time to work with it. He has no zinc powder handy, but heard aluminum may be more effective for reducing anyway. The question is must it be aluminum powder or would some soda cans be good enough? Lame first post, I know, but that's the way it goes sometimes
How bout Al flashing?

The Lone Stranger

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Re: Largescale DMT alcohol cake extraction method?
« Reply #16 on: July 12, 2011, 08:05:36 PM »
antibody2 ....... thanks for the pdf . I read the first paragraph .Been looking for that info for ages and will put it in my collection .

It says what i had thought = that the solvent used extracted a wider range of the contents of the original material than naptha ? Thats why i was thinking water , alcohol or acetone .plus water and alcohol would be cheeper and easyer to get than other solvents .

My mates quark and charm have acsess to some DMT containing material and told me that they will try an extract with acetone . I`ll report back about their results .

As for DMT-nexus thats my opinion to . To many insecure people argueing whos tek is the best when they are mostly nearly the same . I got pissed off and left when a guy called GOD posted his "Slow food tek" = doing the whole extraction only useing a freezer , water and a coffee filter ...... and all the ego wankers started to shout and shoot at him . As far as i know non of them tested what he said and iff its true its the easyest , cheepest and most doable tek i`ve ever seen / posible  ......... would just take weeks to do .

The P.Harmala extract in the foto came from those two mates and i think it was done only with water . Could also have been with a little vinegar as they also tried that . They cant remember .
« Last Edit: July 12, 2011, 08:20:01 PM by The Lone Stranger »

antibody2

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Re: Largescale DMT alcohol cake extraction method?
« Reply #17 on: July 12, 2011, 10:05:25 PM »
@ delafonze19
You might want to do a bit of research on the Al reductions, there are several good write-ups on Rhodium. But in terms of weight, flashing will be very slow as will soda cans. Disposable pie plates or heavy duty Reynolds wrap is a good thickness to work with and will give you a good rxn rate. Al powder will give you a volcano.

But you will need more than just Al. Your Al will need to be activated, perhaps you know this already? You can use Hg salts, Gallium or CuS04 to do this. There was great write up on CuS04/NaCl activation here recently. If I were doing it I would use the CuS04 route, completely OTC and non toxic not to mention inexpensive. You would need much less Al than in that write up

http://127.0.0.1/talk/index.php/topic,1732.msg24202.html#msg24202

shroomedalice

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Re: Largescale DMT alcohol cake extraction method?
« Reply #18 on: July 13, 2011, 12:52:14 AM »
GOD was ok I had a lot of conversations with him on WD and never found him to be anything but honest.

I would say if he said it worked then it did.

The Lone Stranger

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Re: Largescale DMT alcohol cake extraction method?
« Reply #19 on: July 13, 2011, 08:27:09 AM »
Thanks . I think it was probably a different GOD allthough their charakters do sound similar . I tried it to the point of haveing dose of  it . It looked , smelt and tasted right but then i forgot it and it went moldy in the fridge . Being worryed about mycotoxins it got thrown away