STB total failure

[1ce]

Greetings Nexians!

Before I begin let me explain I have a back ground in organic chemistry.
I do not have a degree but I have prepared energetics and my own reagents from scratch for years now. I've done some of the more complicated reactions with very high sucess, asking for help on this is a little embarrassing :/

I've read the FAQs and browsed forums on multiple sites, however I can't find a solution to what could've gone wrong so I'll state my proceedure:

First, a 2000mL borosilicate beaker was filled with distilled water and saturated with 75g NaOH and was allowed to clear and cool to RT. 100g of pulverized MHRB was added to this solution and was agitated for 30 minutes to promote even lysification. I then dropped a stirrbar into the solution and let it mix at a high interval.

After some time had passed I decanted the slurry into an erlenmeyer flask and heated some CH2Cl2 to boiling and added 50mL to the solution. I allowed for the layers to form. I transfered all of the organic layer from the solution and part of the aqeuous layer to an sep. funnel.

I cut the DCM layer leaving just enough with the aqueous layer to avoid contamination and returned everything back to the beaker and continued stirring. I don't have a rotovap and I feared distilling off the solvent under reduced pressure would present an unwanted challenge to collecting crystals so I decided to pour off the solvent layer into a baking dish. Everything can be refined later. I setup a fan and played video games...

I checked back after everything was evapped, to my dissapointment I had no crystals, aside from maybe 10-12 rather small 'freckles', however they fit the profile. When I attempted to remove the precipitate not all was in order: I was scrapping a gummy film off the glass dish and the crystals where lost in the yellow goop. I put this goop into a test tube and heated some heptane. I added boiling heptane dropwise until everything was disolved except for a solid brown chunk I discarded. I poured the heptane off into a 100mm crystalizing dish and stuck it in the freezer overnight.

The next morning to my horror was more yellow resin and some more freckles, none of which would scrape off so I gave up and sanitized my dish. This time to not be defeated I added 50mL boiling naptha into a 2000mL erlenmeyer with my alkaloid enriched water layer. I stired this in thoroughly and after it settled I removed it to a seperatory funnel. I dropped the bottom aqueous layer and kept the top solvent layer. My naptha was now slightly yellow so I had good spirits. By now I was slightly concerned about oxide formation so to keep everything as 'solid' as possible I placed my evap dish over an ice bath to keep the dmt cool and to destroy the soluability of the naptha. I turned the fan on and went to work. When I came back I discovered a couple droplets of alkaloid resin Ithat;s it, 2 extremely small drops) and nothing scrapable. I repeated this for the next coupke days continuously mashing and stirring the mhrb beaker until I was certain of a very thorough lysis.

From 100g pulverized/shredded mhrb my yield was 0.00g of anything. What could I have done wrong? I have never failed an oppenhauer oxidation yet I can't manage an extraction that 'any idiot could do'?

before I dump everything and start over I'd like to try an A/B extraction using a weak acid. Or trying a seperation with chromatography but that would be a waste and rather extreme measure. I think after a vacume filtration an a/b extraction is my best bet..

If anyone catches my errors here I would greatly apriciate any criticism, I'd love to finally cross into the void and begin my journey :/

 

[DansMaTete]

First of all : are you sure your bark is legit ?

Is it from MH ? Is it root's bark ?

 

[1ce]

I feel certain the bark is legit. The freckles have the right crystaline structure, however they never survived harvesting so doing a mp test on them was out of the question. I vaped some of the dirty goo from the first exteaction before treating it with heptane. (To test for activity) and I was treated with a very immediate rush of energy and mental stimulation. I believe this bark is active.

 

[Adjhart]

It seems to me, (someone w no organic chemistry background) that you're way over-complicating things.

Just search the forum for "Cyb's hybrid Salt STB tek", and follow it step for step.

Also, even though my experience is extremely limited, I've not come across any teks that use dichloromethane. Why did you add this?

In my experience, (of extracting beautiful, white crystals on 3 occasions; 3 successful extractions from 3 attempts) vacuum filters and sep funnels are simply not needed to efficiently extract spice.

Maybe just humble yourself with regard to your chem skills and don't reinvent the wheel, ya know?

Best of luck on the next try!:thumb_up:

 

[1ce]

Dichloromethane is susposed to be more selective on pulling more DMT and less 5Meo. I also had more luck with it than naptha >.<

 

[Earthwalker]

Dichloromethane is susposed to be more selective on pulling more DMT and less 5Meo. I also had more luck with it than naptha >.<

I agree with Adjhart don't over complicate things it's might seem complex but it's a simple chem reaction , I would also suggest Cybs hybrid salt TEK as a ATB not STB and with the stuff you have left just try nps but let it mix seperate atleast 4x before freeze precipe !! And if it doesn't work then it would most likely be a bark issue !

 

[1ce]

I know I'm probably way overshooting it but I've done this proceedure countless times with other chemicals without any failures. Sep funnels might not be necessary but they sure are awesome at removing impurities from the solvent. I'll try again with another pull, if anything I can use this failed batch to profile alkaloid content of the bark.

It us definitely mimosa but it could be a less potent variant.

My next extraction I'll use the mentioned tek, although I have acetic, glacial acetic and citric acids to work with I might experiment a little.

 

[1ce]

I had a thought, I think my recent failure had to do with not breaking down the bark enough before adding the NaOH solution. More thorough pulverizing and mashing of the bark would have likely resulted in a realistic yield. I think I found the error of my ways

 

[Deaths Angel]

Evapping leads to goo rather then crystals. try freeze precip

Also try first doing 3x3 hour acid boils and then filter and reduce.

The amount of naptha used seems rather low, again, try doing 3-4 pulls, combine and reduce untill u see crystal formation, then freeze precip. More saturated = better xtals

 

[Adjhart]

I had a thought, I think my recent failure had to do with not breaking down the bark enough before adding the NaOH solution. More thorough pulverizing and mashing of the bark would have likely resulted in a realistic yield. I think I found the error of my ways

From my voracious reading, I would say that an STB done correctly on 100g of average quality pulverized bark, should definitely yield something.

I don't think this was the problem.

It seems like you only did one pull...is that correct? If so, why? Most teks incorporate multiple pulls and for good reason.

I transferred all of the organic layer from the solution and part of the aqueous solution to an sep. funnel

Why only part? Not enough room in the sep funnel? Is it possible you left valuable alkaloid in this solution?


Tips:

Add heat baths to your steps.

If you're set on doing a STB tek, and you want to further lyse in the beginning, just add a boiling solution of 200mL water with 60mL vinegar or similar acidic solution, add to and let sit with pulverized bark for 1 hour, agitating often. Then base.

It's had amazing results here at the Nex for pros and newbs alike.

---

But also, it seems like extra work to do a STB and use a sep funnel, if you're doing multiple pulls (which you should be). As mentioned, a traditional A/B might be better for your setup because you're working with a reduced liquid as your base soup. Much easier to run through a sep funnel 6 times.


Hope this helps

:thumb_up:

 

[1ce]

Deathsanus that might be an issue, I was thinking I'd simply recover whatever evapped and recrystalize from there.

I did 4x pulls leaving the aqueous solution at rt and heating the solvent. I had a 1000mL sep but that's broken ages ago (may she rest in peace). Atm I only have a 250mL sep. That works pretty good if I just suck off the organic layer and a little bit of the aqueous layer to be sure * got all the solvent out. I do want to experiment alot with extractions, particularly with wild phalaris. I've got a good library of solvents and chromat9graphy supplies and I can't wait to dig into it.

Right now though I really just want to experience this molecule. I have a lot of citric acid Lying around. (Literal pounds of granuals). We have a good variety of 'active' plants where I live, and miles upon miles of phalaris. I've found mass amounts here about mhrb, hopefully I can help with some grass extractions down the road.

 

[AffectionateStuden]

for that recrystallization you're doing, acetone might be a good choice. It's worked for me, and is a byproduct of human metabolism. When you extract from Phallaris, you'll defat, correct? Does anyone have an experienced opinion of use of Turpentine as a strong solvent to use during the first couple steps of defatting, to be pulled out by a third defat with Naptha? Further more, does the presence of pink precipitate during basification of acrb signify dmt difinitively? Lastly, if anyone has the attention to donate to my own puzzle of a failed acrb extraction, I would be very grateful, and it may educate other newbies (faq scoured)! The link is: Thank you for being here. Extraction Question! - Introduction Essay - Welcome to the DMT-Nexus

 

[1ce]

White phosphorus is naturally produced by the human body and that was regarded as one of the most toxic substances known to man for nearly 500 years!

Defatting helps to break open the cells in the plant to release dmt for your solvent to puck up. It also removes impurities a majority of the plant matter out of your extraction mix so you can work on isolating dmt as much as possible.

With crystalizations in mind there's a couple things to keep in mind. Soluability of your solvent factors on temperature and how much solvent you have. A solvent will be least soluable when it's at freezing and most soluable at boiling. So to retain much dmt in as little solvent as possible you want to heat it up, as it cools it looses it's soluability and forces the dmt out. It will always retain dmt so maybe keeping your solvent for 1st and 2nd pulls might not be a bad idea because it wont retain the extra dmt, increasing your yield.

Another thing is, keep in mind the boiling point of dmt when you heat your solvent. Heptane boils just a few degrees above dmt's boiling point! You definitly dont want to share your spice with the atmostphere

When you crystalize you wanna do this slowly. Dont just go to the freezer! What happens is the soluability of the solvent is lost at a rate that causes dmt precipitate to form at a speed that traps impurities/solvent and that isn't good at all. Sure the extra alkaloids might not hurt ya but they could take away from the experience. Secondly when the solvent comes out of the freezer (and this goes for solvent trapped in crystals) gets warmed from the room temperature it gains soluability taking your dmt with it. Retaining the solvent for recrystalizations of 1st and second pulls will help you out a little with this as well. In the past I've always taken the product from the cooler, immediately poured off the solvent (and stored it away in an approriate airtight container) for next use. I then evap the remaining solvent over an ice bath or dry ice to keep the solvent as insoluable as possible. This may also help in preventing dmt oxides from forming since you ARE blowing air all over it after all. I don't know how easilly it oxidizes but it's a bonus.

One last thing, you might want to look into getting a sep funnel. They are profoundly awesome at doing washes, extractions and pulls. Then you can seperate out the organic (solvent) or aqueous layer so you're extraction retains it's purity as much as possible. If you look around a decent one wont cost more than a few bucks.. maybe a certain auction site?

I apologize if you already knew all this, but I hope it helps.

Regards, 1ce

 

[Volrux]

After you added the solvent to the basified solution, how long did you let it rest, and how many times did you shake/stir? The ofter you shake/stir, and the longer you let it pull, the more you will extract. What also may help is double boiling the solution while it's pulling. Don't heat it up too much, when it's just a bit warm it's enough.

 

[1ce]

I warmed it and let it mix for about a half hr with an agitation bar so it was thoroughly mixed. I took off the NP layer and a little of the aqueous layer eith a pipette and transfered this to a sep. I didn't heat too much, just enough to boost soluability. I thought I posted saying I had success with some pretty clean crystals, maybe I hit cancel instead..

I believe my biggest failure was allowing a full evap and purifying that with a precip. My yields were great as far as oil is concerned. I just had a hell of a time working with it.