TEK Ethyl acetate approach [CIELO]

[Transform]

same status...

I should follow _Trip_'s advice.
take a look at CITLO. Is it possible to make it with fumaric acid instead of benzoic acid?

Benzoic acid has the advantage of being soluble in toluene, unlike fumaric acid. You'd need to dissolve the fumaric into some solvent like acetone or ipa (and both of those need to be treated with a drying agent to remove water for the crystallisation to work), or you can use an aqueous solution of your acid to recover the target compound, followed by evaporating the water off. In this latter case, it may be better to use a volatile acid like acetic (i.e. white vinegar). That way, excess acid won't end up contaminating your product.

 

[_Trip_]

Read through the lazy salting thread Fractalien there may be more documented combos and failures in there, otherwise you'd have to experiment yourself.

If benzoic acid is hard to find where you live one can make it with sodium benzoate, distilled water and Hydrochloric acid iirc. Sodium benzoate is usually easier to find.

 

[doubledog]

I think that use of benzoic acid is not best option for beginners, as solubility of mescaline benzoate in toluene or xylene seems to be an issue. But preparation of benzoic acid from sodium benzoate is very satisfiying, I would recommend it to everyone - its crystals are very nice and it is a great exercise for any hobby extractor.

 

[FractAlien]

TEK - The benzoic acid tek

I thought about writing a separate post since benzoic acid has not received much attention so far. The greatest benefit of benzoic acid is that it can be used to detect the presence of even very minute amounts of DMT in the NPS. It also allows one to complete the extraction in a single day by...

forum.dmt-nexus.me

Benzoic acid can be easily made from sodium benzoate. Simply dissolve sodium benzoate in hot water and add HCl and benzoic acid will crash out immediately. You can calculate the amount of HCl needed for this reaction, but I'm too lazy to do that, so I just eyeball it, then filter out the left over water, add some more HCl to it and see if anything crashes out. The benzoic acid can further be purified by recrystallization from boiling water. Simply dissolve it in boiling water, let it rest and cool down over night, pour out the water, collect and wash the BA crystals with small amounts of cold water and dry them.

Would it be possible with 30% muriatic acid? Or 85% phosphoric acid?

 

[modern]

Would it be possible with 30% muriatic acid? Or 85% phosphoric acid?

Yes you can make benzoic acid with 30% muriatic acid... IDK phosphoric acid. Did you decide which solvent you are gonna use? If xylene maybe just keep it as diluted hcl acid to salt and allow it to evaporate.

@doubledog mentioned solubility may be an issue so that may not be what you want especially for the first extraction. It may take a while but I'll attempt it myself to test solubility to replace evaporating hcl water to just having a direct precipitate.

 

[Transform]

Would it be possible with 30% muriatic acid? Or 85% phosphoric acid?

Yes you can make benzoic acid with 30% muriatic acid... IDK phosphoric acid. Did you decide which solvent you are gonna use? If xylene maybe just keep it as diluted hcl acid to salt and allow it to evaporate.

@doubledog mentioned solubility may be an issue so that may not be what you want especially for the first extraction. It may take a while but I'll attempt it myself to test solubility to replace evaporating hcl water to just having a direct precipitate.

Phosphoric acid is nonvolatile and therefore not really suitable for this reaction - its tribasicity (three hydrogens) just makes for an additional level of complication, which I won't go into here.

It may be simpler, as modern suggests, to salt from the xylene directly with the HCl as we know that that works.

 

[FractAlien]

Yes you can make benzoic acid with 30% muriatic acid... IDK phosphoric acid. Did you decide which solvent you are gonna use? If xylene maybe just keep it as diluted hcl acid to salt and allow it to evaporate.

@doubledog mentioned solubility may be an issue so that may not be what you want especially for the first extraction. It may take a while but I'll attempt it myself to test solubility to replace evaporating hcl water to just having a direct precipitate.

I will use xylene. It will be great if I can do this directly with diluted HCl! In this case, would form 2 phases, remove the aqueous phase and evaporo for mescaline HCl?

Anyway, I would like to try to make benzoic acid from sodium benzoate. In this case to evolve my DMT extraction.

 

[doubledog]

With xylene, any diluted acid in water will be suitable. Xylene and water will separate in two layers, you just evaporate the water layer. Main issue here is that your product will be contaminated and you will need (or want) to recrystallize it.
HCL salt is quite difficult to re-x, the easiest is sulphate, tartrate is also easy, citrate not so much.

 

[FractAlien]

With xylene, any diluted acid in water will be suitable. Xylene and water will separate in two layers, you just evaporate the water layer. Main issue here is that your product will be contaminated and you will need (or want) to recrystallize it.
HCL salt is quite difficult to re-x, the easiest is sulphate, tartrate is also easy, citrate not so much.

Hey! I think I can buy battery solution (35% sulfuric acid)!
I'll look into re-x mescaline sulfate.

 

[doubledog]

Sulfate is also very rewarding because of its light reflection, it has very distinguishable and beautiful look. I consideder few times in the past to try different acid for change, but then went with sulfuric again just to see it.

 

[modern]

Yes you can make benzoic acid with 30% muriatic acid... IDK phosphoric acid. Did you decide which solvent you are gonna use? If xylene maybe just keep it as diluted hcl acid to salt and allow it to evaporate.

@doubledog mentioned solubility may be an issue so that may not be what you want especially for the first extraction. It may take a while but I'll attempt it myself to test solubility to replace evaporating hcl water to just having a direct precipitate.

So I probably should have first tested salting without drying a bit with sodium sulfate. In any case I pulled with ~200ml of xylene an unknown amount of alkaloids. Decanted and dried. Then I first added 25ml of 'saturated' benzoic acid xylene. BASX but didn't precipitate so I added benzoic acid directly since it seems to be very soluble similar to isopropanol. I added a bit and shook until it all dissolved then after a short period it started to precipitate. There is only a small amount but I started with only a small amount of material and only first pull.

I like this salting but next time I'll leave it in a beaker for easier processing. There was no clouding like with DMT benzoic tek and was similar to BASI where it happens seemingly instantly. I'll preform another pull tomorrow after letting this settle. I'll also attempt using oxalic acid to precipitate. If there is quicker and easier processing I can always do mini a/b for my preferred salt. The no clouding may be due to low content or maybe too dilute since in 230ml?

BTW I remember reading about using ascorbic acid in tests but would always get goo. Is it possible to get salts? I'd imagine concentration and speed of adding the acid would change results but IDK

 

[modern]

S

So I probably should have first tested salting without drying a bit with sodium sulfate. In any case I pulled with ~200ml of xylene an unknown amount of alkaloids. Decanted and dried. Then I first added 25ml of 'saturated' benzoic acid xylene. BASX but didn't precipitate so I added benzoic acid directly since it seems to be very soluble similar to isopropanol. I added a bit and shook until it all dissolved then after a short period it started to precipitate. There is only a small amount but I started with only a small amount of material and only first pull.

I like this salting but next time I'll leave it in a beaker for easier processing. There was no clouding like with DMT benzoic tek and was similar to BASI where it happens seemingly instantly. I'll preform another pull tomorrow after letting this settle. I'll also attempt using oxalic acid to precipitate. If there is quicker and easier processing I can always do mini a/b for my preferred salt. The no clouding may be due to low content or maybe too dilute since in 230ml?

BTW I remember reading about using ascorbic acid in tests but would always get goo. Is it possible to get salts? I'd imagine concentration and speed of adding the acid would change results but IDK

So this morning I put a lab filter to collect the salts... benzoate stuck completely to the glass so I'll need to add water to remove which defeats the point. I'll be trying oxalic acid next since from what I've seen from old reports it becomes a powder rather than crystals which if it doesn't stick to the glass works for me.

EDIT: oxalic acid is pretty much insoluble in xylene so I'm gonna let it sit for a day then wash with isopropanol. Benzoic acid has the benefit of being soluble in xylene so when a precipitate forms its easier to see. There is a tiny amount of solubility 'visually' of the OA in Xylene but hard to tell. Hopefully mescaline oxalate isn't soluble in isopropanol. :S

 

[modern]

The oxalic acid is very insoluble in xylene but there is a difference in appearance when it 'salts' mescaline. It becomes more of a fine powder vs tiny salt balls. So I added a bit excess oxalic acid just to make sure I salt all of the mescaline. There is a mixture of oxalic acid that is unreacted and the mescaline oxalate. So after decanting I added the powder to 99+% Isopropanol and let it sit for a while. There was a noticeable amount of salt (excess oxalic acid) that dissolved in the alcohol and then filtered off the precipitate that remained.
By weight I ended with 120mg which would be around 97mg hcl salt which is in the expected range.
This is easier to salt the xylene than benzoic acid. I'll need some extra steps for use but am satisfied since it didn't stick to the glassware.

I'm letting the alcohol evaporate a little but to see if I can recover a bit more oxalte salt... Maybe freezing will help?

 

[Loveall]

A CIELO video has been posted on YouTube. Some people have asked for something like this so posting it here.

 

[shroombee]

It's interesting that he used an immersion blender for each pull, and that doesn't cause any goo issues. I always stir gently. Perhaps because he had a relatively dry paste, no excess water made it into the extract.

He erroneously said he only had 45 minutes after basing to complete the pulls. Basing time up to at least 72 hours does not affect the pulls or yield. But once the ethyl acetate is added to the cactus paste, the pulls must be completed within ~45 minutes.

 

[Loveall]

It's interesting that he used an immersion blender for each pull, and that doesn't cause any goo issues. I always stir gently. Perhaps because he had a relatively dry paste, no excess water made it into the extract.

He erroneously said he only had 45 minutes after basing to complete the pulls. Basing time up to at least 72 hours does not affect the pulls or yield. But once the ethyl acetate is added to the cactus paste, the pulls must be completed within ~45 minutes.

Yes, with the drier paste (now called dough) it is possible to stir more aggressively.

 

[Loveall]

More updates from the reddit world:

Success "skipping" the dough/paste step. Instead the water was mixed in with a handheld electric mixer in the french press, once incorporated, fridge cold EA was added for the pulls.

No fridge rest, salted directly.

New world record, 32 minutes from powder to xtals. 3.3% yield.

https://www.reddit.com/r/mescaline/s/aAadVzsrlf

 

[shroombee]

Very interesting! He used 95 grams of water for 91 grams of cactus, blended for 15 seconds on the lowest setting with his immersion blender whisk attachment, and then added cold EA. The water content is very low compared to the usual TEK recipe of 130 grams of water for 100 grams of cactus powder (plus up to an additional 130 grams of water to get the correct dough consistency). For comparison, I've always used 300 grams of water for 100 grams of cactus powder (the 69ron paste ratios).

With such a low water content, I wonder if all the mescaline was freebased and pulled? A comparison with identical cactus material using this technique versus the standard TEK would be useful.

 

[Transform]

Very interesting! He used 95 grams of water for 91 grams of cactus, blended for 15 seconds on the lowest setting with his immersion blender whisk attachment, and then added cold EA. The water content is very low compared to the usual TEK recipe of 130 grams of water for 100 grams of cactus powder (plus up to an additional 130 grams of water to get the correct dough consistency). For comparison, I've always used 300 grams of water for 100 grams of cactus powder (the 69ron paste ratios).

With such a low water content, I wonder if all the mescaline was freebased and pulled? A comparison with identical cactus material using this technique versus the standard TEK would be useful.

This is assuming the amounts were reported reliably. Another variable may be the moisture content of the cactus powder - plus there could be a particular low mucilage, high-yielding strain that was suited to his particular approach. Were there any notes regarding the specific cactus used? I wouldn't be surprised to find that TBM was used.
[EDIT: I see now that the plant material was "bridgessi [sic] landrace 329", so my guess about it being bridgesii was at least right ]

 

[Transform]

Revisiting your earlier discussion, @FractAlien …

It seems like a lot of work. I'll try another tek on this batch.

A relevant discussion re-emerged from the archives recently:

Fresh Cacti Strait to DryTEK

Hiya =) Here is the idea : using the ron69 drytek but skipping some steps to gain efficiency. As simple as : putting some fresh (or aged, but still juicy) cuttings of trichocereus in a good blender (vitamix). Then adding the lime strait to this, letting sit for 24h. Let it sit in the sun...

forum.dmt-nexus.me

It appears that fresh cactus + lye + xylene has worked for some, and quetzal7 reported some measure of success with reduced brew + lime + limonene, if you're looking for broad spectrum, rough-and-ready cactus tar: many paths up the same mountain, but some of them get your boots muddier, use more supplies and take longer.