Lye/Limonene/Benzoic acid

[Loveall]

Seeing promising results with this:

- MHRB:Water:Lye paste mixed in 1:1.5:0.25 ratio until homogeneous (a few minutes). First image.
- 5x pulls with limonene 2, 1.6, 1.6, 1.6, and 1.6 parts. 10 minutes stirring, 10 minutes rest. Decanted very easily from the paste.
- Limonene was slightly cloudy. Added a teaspoon of CaCl2 to absorb any water traces (this may not be needed, IDK) and let it rest until clear (a few hours). The settlement stayed at the bottom stuck to the glass and was easy to decant to clear limonene extract . Second image.
- Salted limonene stirring in in 0.03 parts benzoic acid (this is new I believe). Extract became milky white as benzoic acid was dissolved.
- Small white xtals form (3rd picture). They where collected in a filter and washed with ethyl acetate (to remove limonene that can be difficult to evaporate). Dried on coffee filter with squeezing. Result is a white powder (4th picture). Will edit this post with results after collecting.

This run had 50g of MHRB, 75g of water, 12.5g lye, 100g+80g+80g+80g+80g=420g of limonene (- 90%.recovered), 1.5g of benzoic acid. First 3 pulls yielded 1.5g of DMT benzoate candidate. Last two pulls yielded 0.3g for a total of 1.8g of DMT benzoate (1.1g of DMT freebase and 2.2% DMT free base yield). Based on this partition trend, I believe >90% of the DMT have been recovered with the 5 pulls.

Ultimate goal is to make a dilute PG solution with the resulting DMT salt for vaping. Will try to add harmala salts too. Note that some people add small amounts of limonene to their e-juice, so some limonene traces may be fine if I miss any. Safety is not a guarante, doing this for myself and sharing the info, not reccomending people do this or not. Cheers.

 

[Cheelin]

Was hoping for a Citric/EA version of this, but guess I’ll have to add to my ingredient pantry!

 

[Loveall]

Unfortunately, the DMT benzoate candidate is very poorly soluble in PG. Gave up after 1:5:1 ratio of DMT benzoate: PG : Water.

Too bad, this may have been an express lazy route from bark to vapable e-juice salt. So close.

 

[shroombee]

But wait... might this be a quick and easy food-safe method to obtain DMT for pharmahuasca?

Should "MIELO" be reserved for "MHRB in ethyl acetate..." or "Mushrooms in ethyl acetate..."? (And do we think ethyl acetate would work for mushrooms?)

 

[shroombee]

Also, in line with Cheelin's CIELO experiments, is this a good method for quickly determining potency of MHRB?

 

[Loveall]

But wait... might this be a quick and easy food-safe method to obtain DMT for pharmahuasca?

Should "MIELO" be reserved for "MHRB in ethyl acetate..." or "Mushrooms in ethyl acetate..."? (And do we think ethyl acetate would work for mushrooms?)

If one wants a DMT salt as the final product, I would say this would be the fastest method I'm aware of because it simplifies the salting step (no FASA preparation/management). Bit first, O would want to send the product form analysis to be sure it is relatively pure DMT as it's appearance suggest. Not food safe cause of lye, but the limonene is and that tis near the end. I tested a small batch with lime and it also seems to work, but I went with lye in case it helps yields by breaking down the bark, but not sure if it does though.

I tried ethyl acetate for MHRB and it didn't work for me. I tried mushrooms to and it did not work.

I do wanna try mushrooms again (ethyl acetate did not work), but this time with baking soda, limonene or IPA and benzoic acid.

Also, in line with Cheelin's CIELO experiments, is this a good method for quickly determining potency of MHRB?

I don't see why not, would want to confirm composition and purity with MS.

Cheers

 

[shroombee]

If one wants a DMT salt as the final product, I would say this would be the fastest method I'm aware of because it simplifies the salting step (no FASA preparation/management). Bit first, O would want to send the product form analysis to be sure it is relatively pure DMT as it's appearance suggest. Not food safe cause of lye, but the limonene is and that tis near the end. I tested a small batch with lime and it also seems to work, but I went with lye in case it helps yields by breaking down the bark, but not sure if it does though.

There is food safe lye advertised, so I guess it's food safe? But if lime works as well, I would use lime for the safety.

Assuming the end product is what we think it is, this should be a TEK. I personally don't vape DMT, rather I use it in salt form for pharma. And I have a potential use with a Parkinson's patient who would be more comfortable with oral ROA rather than vaping.

I tried ethyl acetate for MHRB and it didn't work for me. I tried mushrooms to and it did not work.

I do wanna try mushrooms again (ethyl acetate did not work), but this time with baking soda, limonene or IPA and benzoic acid.

Sorry I didn't mean to bring ethyl acetate and MIELO into this discussion, as this thread is about Limonene as the solvent.

Still interested in whether we can precipitate psilocybin. What salts did you try with mushrooms and ethyl acetate?

 

[Loveall]

If one wants a DMT salt as the final product, I would say this would be the fastest method I'm aware of because it simplifies the salting step (no FASA preparation/management). Bit first, O would want to send the product form analysis to be sure it is relatively pure DMT as it's appearance suggest. Not food safe cause of lye, but the limonene is and that tis near the end. I tested a small batch with lime and it also seems to work, but I went with lye in case it helps yields by breaking down the bark, but not sure if it does though.

There is food safe lye advertised, so I guess it's food safe? But if lime works as well, I would use lime for the safety.

Assuming the end product is what we think it is, this should be a TEK. I personally don't vape DMT, rather I use it in salt form for pharma. And I have a potential use with a Parkinson's patient who would be more comfortable with oral ROA rather than vaping.

I tried ethyl acetate for MHRB and it didn't work for me. I tried mushrooms to and it did not work.

I do wanna try mushrooms again (ethyl acetate did not work), but this time with baking soda, limonene or IPA and benzoic acid.

Sorry I didn't mean to bring ethyl acetate and MIELO into this discussion, as this thread is about Limonene as the solvent.

Still interested in whether we can precipitate psilocybin. What salts did you try with mushrooms and ethyl acetate?

Agreed, lye can be food grade. I believe germans use it for pretzels after it reacts with the dough in water. In general we don't consider it food safe here by convention because it is corrosive in pure form. I guess it is an arbitrary convention in a way (?).

I can reccomended experimenting with the MHRB/lime/limonene/benzoic acid. I got what looks like very pure DMT benzoate very easily after pulling from the lime paste. Probably want to powder the MHRB very well and/or freeze/thaw since lime won't break down the bark (?). Anyway, this should be a very direct path to get relatively pure salt from what I've seen, but we need an MS to say this is not experimental and pending confirmation.

With mushrooms, I tried heating a citric acid paste to convert to psilocin, then based with sodium bicarbonate to convert to neutral, charge, pulled with EA, salted with citric and fumaric. Got oils, no xtals. Never tested if the oil was active, just gave up at this point.

 

[Cheelin]

I’m gonna be working on the bark maceration issue soon, freeze-thaw is so old school.

 

[Loveall]

Update: since the DMT benzoate candidate did not dissolve in PG , dumped the experiment in water, based, pulled with naphtha, and freeze precipitated.

Got 0.95g of DMT FB. Would be 1.1g based on moles or DMT Benzoate, but 0.95g makes perfect sense cause I only pulled a couple times and the naphtha is new (wasn't evaporated so a few mg of product remain in it and will be present on the next extraction).

I think this confirms that relatively pure DMT benzoate was indeed the product obtained in the original post. I don't think an analysis is needed. Cheers.

 

[shroombee]

Update: since the DMT benzoate candidate did not dissolve in PG , dumped the experiment in water, based, pulled with naphtha, and freeze precipitated.

Got 0.95g of DMT FB. Would be 1.1g based on moles or DMT Benzoate, but 0.95g makes perfect sense cause I only pulled a couple times and the naphtha is new (wasn't evaporated so a few mg of product remain in it and will be present on the next extraction).

I think this confirms that relatively pure DMT benzoate was indeed the product obtained in the original post. I don't think an analysis is needed. Cheers.

Cool. Thanks for the update. Is this the typical yield you would expect from this source material?

 

[Loveall]

Yep, when it all goes well I'm slightly above 2%. Many different TEK/approaches converge to this number with the material I have as long as there are no issues.

 

[_Trip_]

With mushrooms, I tried heating a citric acid paste to convert to psilocin

Loveall isn't psilocybin converted to psilocin in the liver via (ALP) alkaline phosphatase enzyme?
So to convert to psilocin couldn't one buy alkaline phosphatase and use that or could phosphoric acid perhaps work?

Just wondering, I could be off the mark here.

 

[Loveall]

With mushrooms, I tried heating a citric acid paste to convert to psilocin

Loveall isn't psilocybin converted to psilocin in the liver via (ALP) alkaline phosphatase enzyme?
So to convert to psilocin couldn't one buy alkaline phosphatase and use that or could phosphoric acid perhaps work?

Just wondering, I could be of the mark here.

I guess so, not sure. 1h in mild acidic conditions and heating to 70C for a few minutes will do it for according to Casale's procedure (attached).

 

[shroombee]

Yep, when it all goes well I'm slightly above 2%. Many different TEK/approaches converge to this number with the material I have as long as there are no issues.

MILLO = MHRB In Limonene Leisurely Over-the-counter.

 

[_Trip_]

Obviously acetic acid works according to that paper, would be worth testing a number of other acids then. Fitting in with the whole ALP makes me think phosphoric acid might be a good candidate too.

It's an interesting paper I wouldn't have thought dephosphorylating psilocybin and then crystalizing psilocin would be a bit harder than that.

Good find.

 

[Loveall]

Obviously acetic acid works according to that paper, would be worth testing a number of other acids then. Fitting in with the whole ALP makes me think phosphoric acid might be a good candidate too.

It's an interesting paper I wouldn't have thought dephosphorylating psilocybin and then crystalizing psilocin would be a bit harder than that.

Good find.

Benzyme found that paper. Years ago we had some success pulling with xylene and salting with FASA. Psilocin fumarate Xtals were obtained according to the MS, but the yields were small and xylene is horrible to work with . I still have some of those xtals in my garage. They haven't changed over time at least in appearance.

Preserving the psilocin from degradation during the extraction process may be very important. Casale doesn't mention yields I believe. I think having vitamin C in the process could be important before basing with bicarbonate.

 

[_Trip_]

Sounds like some experimenting will be in order once the next season kicks in.

 

[Jan e Kharabat]

- Salted limonene stirring in in 0.03 parts benzoic acid (this is new I believe). Extract became milky white as benzoic acid was dissolved.
- Small white xtals form (3rd picture). They where collected in a filter and washed with ethyl acetate (to remove limonene that can be difficult to evaporate). Dried on coffee filter with squeezing. Result is a white powder (4th picture). Will edit this post with results after collecting.

how did you add benzoic acid in limonene? dissolved in hot water? or directly in limonene? I read that benzoic acid is also soluble in hexane. If so, one could directly dissolve it in Naphtha to crash out DMT benzoate no?

 

[Loveall]

- Salted limonene stirring in in 0.03 parts benzoic acid (this is new I believe). Extract became milky white as benzoic acid was dissolved.
- Small white xtals form (3rd picture). They where collected in a filter and washed with ethyl acetate (to remove limonene that can be difficult to evaporate). Dried on coffee filter with squeezing. Result is a white powder (4th picture). Will edit this post with results after collecting.

how did you add benzoic acid in limonene? dissolved in hot water? or directly in limonene? I read that benzoic acid is also soluble in hexane. If so, one could directly dissolve it in Naphtha to crash out DMT benzoate no?

Yes, I added the benzoic acid granules (3% by weight of root bark).

Yes, you can try to add benzoic acid to hexane, it should dissolve. As long as it reacts with DMT you will should get DMT benzoate to precipitate. I haven't tested that since with napthata I freeze precipitate to get FB.