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Ethyl acetate approach [CIELO] Options
 
orchidist
#1121 Posted : 3/9/2022 5:22:08 AM

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Some interesting developments.

I collected the decanted solvent from my fumarate crystals, split it in two portions as described above.

The one which I did not wash remained clear on addition of the citric acid, however, it looks like maybe some additional non-citric acid crystals have formed. Will wait overnight to give it time to be sure all CA should be dissolved.

The one I washed with sodium carbonate actually clouded up a tiny bit when I added citric acid. That'll be very interesting to observe come morning.
 

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Loveall
#1122 Posted : 3/9/2022 9:23:59 AM

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orchidist wrote:
Cheelin wrote:
Maybe this is better for Loveall, but why wouldn’t you, as I mentioned earlier, drop an M-fumerate crystal into the citric jar and see if that drives crystallization?


Sorry, I meant to reply to that but I got scattered. I do think it's a good idea, and I tried it, but unfortunately it had no effect on the already oiled jar. I have one more portion of unsalted extract set aside. I wonder if I adding a couple seed crystals at the very start might help.

I'm going to hold off on that while I work on explore whether I can crystallize by converting the fumarate to the citrate. I was hoping to hold off on more citrate experiments until I could get results from Solaris, but it looks like they're not accepting new samples until at least July. I requested to be put on their mailing list, if they maintain one.

Do we know of any alternatives to Solaris?


Another analysis place is Energy control (contact Endlessness), based in Europe.

Let's see what you get with current tests. We can ask benzyme about the Solaris queue if needed.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
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orchidist
#1123 Posted : 3/11/2022 4:11:15 AM

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Sorry for the delay, I will get in touch with endlessness.

Turned out the tiny quantity of solids at the bottom of the jars where I added citric acid to the previously fumaric salted solvent was not enough to show anything on my TLC plate. Probably should've just dropped some Marquis reagent on it instead. Hindsight...

I only used 100ml of solvent for this, but I have a couple liters of FA salted solvent to examine this weekend, so it's possible I may end up with enough material to run a TLC.

With regards to converting some of my fumarate back to citrate, I am hesitant to risk any more yield loss if I can help it. Fumaric acid works great for me. Still very curious to know what else is in this stuff that may be interfering, so hopefully we can get some mass specs!
 
Loveall
#1124 Posted : 3/11/2022 8:19:53 AM

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Ok.

Another possible easy test would be to add fumaric to the solvent crashed with citric. Have you tried that yet?
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
orchidist
#1125 Posted : 3/13/2022 12:50:14 AM

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Loveall wrote:

Another possible easy test would be to add fumaric to the solvent crashed with citric. Have you tried that yet?


Done as of last night! Keeping an eye on it. So far no change.

Found something pretty interesting in one of my jars of used citric salted solvent today. Oily droplets that looked exactly like M. It solidified when washed with fresh EA, just like the M oil too. I assumed it was product that had escaped while decanting, but it has no reaction to Marquis reagent and tastes sour. No bitterness.
 
orchidist
#1126 Posted : 3/13/2022 2:56:15 AM

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I haven't been recording yield % for most runs since I had been dividing the solvent for various trials. Those crystals were combined into one filter funnel. I did a full scale 100g run and got 700mg of fumarate, which corresponds to 863mg citrate, 452mg of freebase. That'd be 0.452% mescaline by dry weight, which seems reasonable according to this erowid article
 
Cheelin
#1127 Posted : 3/13/2022 3:24:40 AM

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Thanks.

I think 1% is considered ok, bragging rights start higher; though, unlike dosage, most people don’t say what salt basis they are using.
 
orchidist
#1128 Posted : 3/13/2022 3:48:08 AM

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Yeah, not the most exciting result for sure, but right now I'm happy I got anything

It would for sure be most useful if everyone reported their yields in terms of the freebase, not whatever salt was formed so we could compare apples to apples. But now that I've got a baseline and procedure that is working for me, I can at least compare directly against myself and look for consistency in the yield. If there's a lot of variability, probably my fault, otherwise, probably unimpressive starting material.

Eventually I'll have my own harvestable columns and not have to rely on a third party for my material.
 
orchidist
#1129 Posted : 3/13/2022 5:04:19 AM

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Has anybody directly compared their yields of fumarate vs citrate for the same material? There are some properties of fumaric acid that make me think the formation of a dimescaline salt may be more probable than with citric acid. (Fumaric acid is about 2x as strong as citric acid, and its symmetry may be favorable for crystallization)

If that's the case, 700mg fumarate would be equivalent to 1049mg of citrate, or 549mg of freebase.
 
_Trip_
#1130 Posted : 3/13/2022 5:43:18 AM

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I believe Loveall has, there's a topic on here somewhere but if you check the CIELO tek wiki page he has written them in there towards the bottom of the page.

https://www.dmt-nexus.me...p;m=1136570#post1136570 here's the results it's in this thread.
Disclaimer: All my posts are of total fiction.



 
orchidist
#1131 Posted : 3/13/2022 2:09:56 PM

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_Trip_ wrote:
I believe Loveall has, there's a topic on here somewhere but if you check the CIELO tek wiki page he has written them in there towards the bottom of the page.

https://www.dmt-nexus.me...p;m=1136570#post1136570 here's the results it's in this thread.


Thank you! That seems pretty convincing that the fumarate is a 1:1 salt. I'm very surprised that the malate would be 2:1 while others are not, considering the 2nd pKa is quite a bit weaker than either citric or fumaric acid.

Glad to finally have a baseline yield for what I'm working with. Hopefully it can be pushed up. If not, at least my yield is in range of published values.

Found a more thorough compilation of data in Trout's notes
 
Loveall
#1132 Posted : 3/13/2022 5:27:21 PM

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orchidist wrote:
_Trip_ wrote:
I believe Loveall has, there's a topic on here somewhere but if you check the CIELO tek wiki page he has written them in there towards the bottom of the page.

https://www.dmt-nexus.me...p;m=1136570#post1136570 here's the results it's in this thread.


Thank you! That seems pretty convincing that the fumarate is a 1:1 salt. I'm very surprised that the malate would be 2:1 while others are not, considering the 2nd pKa is quite a bit weaker than either citric or fumaric acid.

Glad to finally have a baseline yield for what I'm working with. Hopefully it can be pushed up. If not, at least my yield is in range of published values.

Found a more thorough compilation of data in Trout's notes


It may have more to do with the solubility thank the pKa. If 1:1 malate is soluble in EA it may react further and crash at 2:1. Not sure, just speculating on the meaning behind the measurements I got, could be wrong.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
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Cheelin
#1133 Posted : 3/14/2022 12:43:41 PM

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Metta-Morpheus wrote:
Hi Cheelin,

I have gone thru and deleted your one word/emoji posts. These are useless and just take up space. Please refrain from further one word responses.

Metta-Morpheus



Petty!


Thanks Loveall et al, great tek!
 
Voidmatrix
#1134 Posted : 3/14/2022 12:51:11 PM

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Cheelin wrote:
Metta-Morpheus wrote:
Hi Cheelin,

I have gone thru and deleted your one word/emoji posts. These are useless and just take up space. Please refrain from further one word responses.

Metta-Morpheus



Petty!


Thanks Loveall et al, great tek!


It's not petty eliminating frivolity.

One love
What if the "truth" is: the "truth" is indescernible/unknowable/nonexistent? Then the closest we get is through being true to and with ourselves.


Know thyself, nothing in excess, certainty brings insanity- Delphic Maxims

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Question everything... including questioning everything... There's so much I could be wrong about and have no idea...
All posts and supposed experiences are from an imaginary interdimensional being. This being has the proclivity and compulsion for delving in depths it shouldn't. Posts should be taken with a grain of salt. πŸ‘½
 
downwardsfromzero
#1135 Posted : 3/17/2022 9:30:28 PM

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orchidist wrote:
Yeah, not the most exciting result for sure, but right now I'm happy I got anything

It would for sure be most useful if everyone reported their yields in terms of the freebase, not whatever salt was formed so we could compare apples to apples. But now that I've got a baseline and procedure that is working for me, I can at least compare directly against myself and look for consistency in the yield. If there's a lot of variability, probably my fault, otherwise, probably unimpressive starting material.

Eventually I'll have my own harvestable columns and not have to rely on a third party for my material.

If it's comparing apples with apples we want, the reference standard should, clearly, be the malate salt. Big grin
[chemistry joke - check the etymology of malic acid if you don't get it Very happy ]

Malate is, to a large extent, the salt form we can expect in the cactus - but really I'd like to bump that link to the salt equivalent calculator spreadsheet: {which will be here when I can find it, unless someone beats me to it ↓↓↓}
[EDIT: Orchidist found it - thanks and well done - and I've put the link here as well. And a few posts further on you'll find my update including mescaline citrates. It would be simple to add malates to the list as well.]




β€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
orchidist
#1136 Posted : 3/18/2022 1:52:38 AM

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downwardsfromzero wrote:
orchidist wrote:
Yeah, not the most exciting result for sure, but right now I'm happy I got anything

It would for sure be most useful if everyone reported their yields in terms of the freebase, not whatever salt was formed so we could compare apples to apples. But now that I've got a baseline and procedure that is working for me, I can at least compare directly against myself and look for consistency in the yield. If there's a lot of variability, probably my fault, otherwise, probably unimpressive starting material.

Eventually I'll have my own harvestable columns and not have to rely on a third party for my material.

If it's comparing apples with apples we want, the reference standard should, clearly, be the malate salt. Big grin
[chemistry joke - check the etymology of malic acid if you don't get it Very happy ]

Malate is, to a large extent, the salt form we can expect in the cactus - but really I'd like to bump that link to the salt equivalent calculator spreadsheet: {which will be here when I can find it, unless someone beats me to it ↓↓↓}


Love it Big grin My other hobby gives me tons of exposure to etymology, especially of the botanical sort.

And a calculator would definitely be great, I made my own in the spreadsheet I've been using to proportion ingredients for this tek. At some point, I'd love to spend some time writing up some calcualtors in javascript.

Anyway, Loveall, I forgot to share that I made saturated solutions of my citric acid in EA and water, no residues to speak of.

I spent some time in the references on the CIELO wiki, particularly the mycotopia thread regarding transparent tacky product from bridgesii. The product described there seems a whole lot like what I got. That thread continued, and it looks like it might not just be bridgesii, but more generally powder made from whole cactus. I have no way to be completely certain, but I wouldn't be surprised at all if all the powders I got use the entire cactus. That would account for the lower yields too.


 
orchidist
#1137 Posted : 3/18/2022 4:17:19 AM

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dfz, I think I found the conversion spreadsheet here. Looks great!
 
Loveall
#1138 Posted : 3/18/2022 5:37:22 PM

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Orcjidist, I used whole cactus powder earlie on and got xtals. However, there could be difference s in drying, cactus, etc.

Have you always gotten goo using citric acid with the other whole cactus powders?

Anyone else get xtals with whole cactus powder? If yes, how did they dry it?

Anyone get goo with outer skin after feeling they got the process done right?
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
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πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
downwardsfromzero
#1139 Posted : 3/18/2022 8:13:23 PM

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orchidist wrote:
dfz, I think I found the conversion spreadsheet here. Looks great!

Nice one; a bit further down that thread there's an updated spreadsheet with mescaline citrate included and sooner or later I/someone could add malates as well.




β€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
downwardsfromzero
#1140 Posted : 3/18/2022 8:30:34 PM

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Some points for consideration, from a new member here.
Nemooo wrote:
This is for the Ethyl acetate approach thread by Loveall. I can't seem to post in there.

Great job on coming up with a greener and faster method that appears to give high purity product!

A few suggestions:
1) Dry the solvent before trying to precipitate the alkaloid salts:
- I saw some effort to dry the ethyl acetate, but CaCl2 is generally not compatible with amines or esters as they can form a complex with it, it can also be slow and finicky.
- K2CO3 is your best bet, compatible with both amines and ethyl acetate. Only use just enough and give it time to do its job. Molecular sieves are a possibility too.
- A dry solvent will make things more reproducible and will lead to faster crystallisation and also should avoid the formation of the biphasic "oil" some have seen. The "oil" appears to be a very saturated solution of alkaloid salt and acid, the addition of the acid in the presence of water in the solvent means the more polar compounds can form aggregates and eventually separate out due to the increase in polarity/ ionic nature. The fact they are in solution also means the stoichometry of the alkaloid salt could vary.

2) Dissolve the solid acid of choice (citric, fumaric etc) in ethyl acetate first, then add this to the ethyl acetate extract.
- This, providing the extraction solvent is dry enough, will mean the amount of acid can more accurately titrated (yes excess acid is soluble in ethyl acetate, but if a biphasic system develops it will also partition itself between the aqueous and organic layers complicating things).
- The ethyl acetate may need to be heated or sonicated to get more acid to dissolve but this is ok, just let it cool before adding to the extract.

3) Consider trying succinic acid:
- Fumaric acid is a Michael acceptor and there are cases in the literature recording amines reacting with it in this way. Probably fine most of the time, but should a solution need heat sterilisation that could be a problem.

4) Do an A/B extract on the residue to prove all alkaloids have been extracted.
- I think you should do this to confirm it gets all the alkaloids.

5) Melting point
- Do a melting point.This will tell you how pure it is.
- Popping or change in crystal structure prior to melting would indicate solvent or water or crystallisation/ hydrate.
- Otherwise more spectroscopic data to show it is clean and doesn't need recrystallisation. That Mass Spec you showed doesn't say how it was obtained, and doesn't tell the whole story. Im guessing it was run in positive mode only so no acids present?

6) Recrystallisation.
- Would be great to see some solubility information on the citrate/ fumarate/ succinate and also recrystallisation.





β€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
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