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Citric of Fumaric Acid for bufo A/B? + other q's Options
 
soulfood
#1 Posted : 9/15/2009 1:40:48 AM

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Ok I've got a little free time coming up and I am once again going to face my nemisis that is the bufotenine extraction. As I have little oppotunity for this kind of thing these days I really want to get it right this time. I've done lots of reading here and there trying to figure out what's gone wrong in previous attempts and generally finding out better ways of working this molecule. I'm pretty sure there's nothing on this site about bufotenine I haven't read at least once.

This is going to be the procedure I am planning to use this time round with comments and questions here and there for the sections I am not sure about.

1. Toast seeds at 500f until the popping stops.

2. Grind up seeds to a fine powder

3. Run acetone through seeds until acetone comes out clear.

Ron reports his SWIM having good results when using DCM for his defats. What is the difference if any when using DCM instead of acetone? I can't acquire DCM, but I have also read of people using room temperature xylene for this part of the process. I always figured acetone to be a much stronger solvent than xylene. Basically other than reading about relevant alkaloids solubility with the common alkaloids known to this forum I have zero knowledge on solvents.

4. Basify material with sodium carbonate/air dry.

5. Rinse material thoroughly with acetone.

6. Acidify acetone(FASA/CASA). Collect precipitates.

This is my main point of interest here really. I always used fumaric acid at this point, because I figured the resulting material would be much easier to handle. However I recall reading somewhere that it is better to use citric acid for bufotenine, but there weren't any details on why. If I rinsed either end product with acetone could I expect different levels of purity in either product?

I understand the two substances have a very similar level of acidity, but could there be some other property that makes the two substances different?

Also what are the advantages of evapping the acetone to a smaller volume before acidifying, besides a more manageable quantity?


7. Basify extract with sodium carbonate.

Would it be a good idea to do this process in solution rather than the dry/paste method? I know I don't have access to a suitable solvent for extracting bufotenine from water, but I'm interested if there are any toxins that would be more water soluble than bufotenine if I just shoot the ph high enough to basify the bufotenine?

8. Dry/heat in the oven.

This is the first heating that I will be using in the base state. I know most people toast the seeds again like they were preparing a cebil snuff before they start the rest of the extraction, but are there any disadvantages in waiting until this stage to toast the extract?

9. Pull with acetone/evap

10.... Well hopefully by this stage I will be looking at something worth purifying and will try anything but a limonene boil.


Only other thing is, has anyone acheived 95% pure + bufotenine when not using argentinian seeds?

So hopefully all you beautiful, kind and smart people Smile will let me know what you think. I know this sort of thing has been asked many times before so thanks to those who made it this far. I'll probably be starting this up in just under a week so I'll post my updates here.

This time Smile here's hoping.
 

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soulfood
#2 Posted : 9/15/2009 11:19:45 PM

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Ok.. think I found out what I was talking about with the citric acid thing. I guess that it's just way more soluble in acetone.

I'm thinking about embarking on a search for DCM.
 
Infundibulum
#3 Posted : 9/15/2009 11:50:04 PM

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soulfood wrote:
Ok.. think I found out what I was talking about with the citric acid thing. I guess that it's just way more soluble in acetone.

Yup, making CASA is way easier; there's also another thing re CASA vs FASA. Anadenanthera colubrina have traces of dmt and dmt citrate is somewhat soluble in acetone. Acidifying with CASA means that one loses the dmt and keeps the bufo.

On the other hand, FASA will got the dmt as well.

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
amor_fati
#4 Posted : 9/18/2009 5:01:15 AM

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SWIM found the CASA to be a little tricky the first time. The solution will cloud up beautifully, but the precipitates will settle as a red goo at the bottom and look like next to nothing (frustrating for the inexperienced). However one would notice the sides of the container to be covered in a goo precipitate as well. When the container is thoroughly washed and the wash water collected and evaporated, it will yield a hard resin that, when scraped up (with some difficulty) will turn out much heftier than it first appeared.

SWIM's freebase turned out a bit tarry, so he did the limonene boil, which he found a little cumbersome, but bearable and useful. He didn't manage to do it the way he had expected. SWIM managed to clean out all the tar that simply wouldn't dissolve in boiling limonene, but that's about all he managed to do. The freebase yield after that was a hard slightly sticky (like hard rock candy) resin that smokes nicely in his machine-style lab bubbler.
 
soulfood
#5 Posted : 9/18/2009 10:42:14 PM

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Did you use heat to evap the water after rinsing out the bufo citrate or did you let it air dry?
 
amor_fati
#6 Posted : 9/19/2009 2:59:38 AM

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soulfood wrote:
Did you use heat to evap the water after rinsing out the bufo citrate or did you let it air dry?


155F in a food dehydrator.
 
soulfood
#7 Posted : 9/19/2009 3:53:54 AM

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I've just boiled some seeds in ph3 citric acid solution then slowly boiled the water off in an oven at 90C. Got a sticky mess, but it's not runny. I think it's probably highly contaminated with citric acid... should have used vinegar. Oh well. Just waiting for some acetone then I'll get the excess out then proceed as though I was doing the standard acetone tek.

I like it that I've got the actives out without using 1L of acetone though... very nice.
 
amor_fati
#8 Posted : 9/19/2009 3:48:26 PM

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It's definitely going to be fairly contaminated with citric acid. Citric acid doesn't always seem to dissolve into acetone very easily or fast, but will dissolve completely in the right concentration. When SWIY purifies it, be sure to give it plenty of stirring and time and keep the container sealed to avoid moisture contamination (considering it may take some time). SWIM wonders if it would be possible to purify it with water, if the XlogP's differ enough.
 
soulfood
#9 Posted : 9/19/2009 6:53:51 PM

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I've done a bit of defatting using 500ml DCM. Is citric acid soluble in DCM? I probably could have done a bit more defatting but I hate working with that stuff, but the solution seems a bit less dark now. I'm going to revert back to the standard acetone tek.
 
soulfood
#10 Posted : 9/21/2009 12:18:35 AM

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amor_fati wrote:
It's definitely going to be fairly contaminated with citric acid. Citric acid doesn't always seem to dissolve into acetone very easily or fast, but will dissolve completely in the right concentration. When SWIY purifies it, be sure to give it plenty of stirring and time and keep the container sealed to avoid moisture contamination (considering it may take some time). SWIM wonders if it would be possible to purify it with water, if the XlogP's differ enough.


Yeah it tastes very fizzy. I'm going to do a couple of day long soaks in acetone, so hopefully that will sort things out.

Sorry, I don't really understand the mechanics of the XlogP. The citric acid didn't come out with some 500ml's worth of defats with DCM, so I suppose if I basify, then pull that with DCM it may leave the citric acid in there. I'm not a fan of DCM though.
 
 
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