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Preparation of crystalline THCA

@greenman @skyhighler it is due to purity. I previously posted a paper showing the kinetics of decarboxylation. In that paper they refer to two paths to decarb: naturally occurring acid catalysis, or the high energy path of the keto-enol form.

In the trichome and most extracts, there are naturally occurring acids. These acids cause Decarb to occur through an intermediate interaction between the acid and THCA. This allows decarb to occur at lower energy and is moved forward with things like added light energy or added energy from naturally occurring oxidation.

Once THCA is isolated and other naturally occurring acids are removed, this cannot occur. This leaves the only decarb pathway occurring at much higher energy then the isolated crystals will see at room temp or even exposed to light. The pathway left is the keto-enol form which will take higher energy, i.e added flame, enail, oven, etc.
 
@greenman @skyhighler it is due to purity. I previously posted a paper showing the kinetics of decarboxylation. In that paper they refer to two paths to decarb: naturally occurring acid catalysis, or the high energy path of the keto-enol form.

In the trichome and most extracts, there are naturally occurring acids. These acids cause Decarb to occur through an intermediate interaction between the acid and THCA. This allows decarb to occur at lower energy and is moved forward with things like added light energy or added energy from naturally occurring oxidation.

Once THCA is isolated and other naturally occurring acids are removed, this cannot occur. This leaves the only decarb pathway occurring at much higher energy then the isolated crystals will see at room temp or even exposed to light. The pathway left is the keto-enol form which will take higher energy, i.e added flame, enail, oven, etc.


Thanks for the explanation!
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
I don't recall a discussion of the Guild's patent application, has anyone found it?

"Our proprietary, patent-pending technology enables us to isolate high levels of THCa to create one of the purest extracts in the world - THCa Powder." http://www.guildextracts.com/products/
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Don't get your hopes up...

"How Come I Cannot Find Patent Pending Info?

Posted on Sep 30, 2011 by attorney Danton Mak

This is not an unusual case: you see a "patent pending" notice on your competitor's product. Yet when you go to the US Patent Office website, you can find no information about the pending patent under the competitor's company name. How come?

Utility patent applications are published generally 18 months from the earliest priority date claimed in the application. Design patent applications are not published at all. Before publication, the file is kept secret and 3rd parties cannot get information on the application. If you do not find anything under the company name, some of the possiblities could be:

It has been less than 18 months;

The pending application is a design patent application;

You looked in the wrong place (there are 2 separate databases, one for issued patents, and one for published applications);

It is also possible that the applicant requested no-publication (generally the applicant has to forego foreign filing of the application); or

Since all U.S. patent applications are filed in the name(s) of the inventor(s) individually, searching by company name would not produce results if there was no assignment of the application to the company.

One plausible alternative (if you still cannot find the information) would be to order a right to use search. But that is typically quite expensive (thousands of dollars, depending on the technology), and can only be justified for major product lines.

Danton K. Mak

Sheldon Mak & Anderson PC

100 Corson Street, Ste 300

Pasadena, California 91103-3842

(T) 626.796.4000

(F) 626.795.6321

E-Mail: danton@usip.com

(Direct Line) 626-356-1288

(SKYPE) dantonm

(Home Page) http://www.usip.com"

https://www.avvo.com/legal-guides/ugc/how-come-i-cannot-find-patent-pending-info
 
I'm not a patent expert but from my view these techniques have been made public through this site. We have covered the base techniques to produce in it atleast 3 ways. It's also basic chemistry and purification of THCA has been covered in other literature.

They may get the patent through the patent office not seeing anything else but if taken through the courts I don't think it'll hold much weight.

This is how MAPS has protected MDMA from specific use patents.

It's a smart move on Guilds part, however. If they do receive the patent, they could sell it to a company like GW and easy make alot of money very quickly.
 
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99.99 thca

New member
Could pangea o weedalcoholic explain it carefully? Ive been reading everything for the last few months, in europe we cant have access to this medicine and i want to make my own, ive noticed that the only way to make it is with column chromatography or acid base extraction, once you have it for obtain the crystals you must use the crystallation technique.... This is very helpful but.... Could you guys explain properly again for the people that are studying the terms with this sustance? I dont know if its better to xtract bho from live resin and try to make a a/b extraction or with normal winterized oil is good to do it

Thanks a lot for this post guys ive been reading you for few months and the account was created for this reason, im an european patient that can have access to this, is not possible in europe, i only want to learn from you mates, this wonderful plant means a lot for me. Thanks for your compression boys
 

99.99 thca

New member
I already got this:

- decarboxylation does not occur in basic conditions but will in acidic conditions
- the base is used to "pull the hydrogen off" of the -COOH of the THC-a. Then once neutralized with an Acid "adding H(+) back to the COO(-), THC-a should precipate out. Sodium bicarb is a weaker base so the idea is it avoids extraction of phenolics but dilute NaOH would work as wellp.

I have an example of a extraction but i dont know the measurements even i dont know if its good:

- Add 50 g grass/liter petroleum ether or benzeme; soak 12 h with occasional shaking; filter and extract petroleum ether 3 times with a solution contaning 5% NaOH and 5% Na2SO3.
- Acidify the aqueous extracts with cold dilute sulfuric acid, acid extract with ether or chloroform which is dried evaporated in a vacuum to yield the cannabidiolic acid.
- THC and cannabidiol remain in the petroleum ether which can be dried and evaporated in a vacuum and the residue added to grass.

Another one:

- Extract three times with charcoal lighter or any lighter or any light aliphatic mix around one mason jarfull or fresh fan leaves or higher quality.
- Prepare solution of 1g NaOH to 250 g H2O.
- Combine the nonpolar and lyewater vigorously, forming sodium thc acid sal.
- Separate layers, non polar can be evapped to yield ok honey oil.
- Acidify aqueous solution with sulfuric or far low pH.
- Add small amount of non polar, shake and remove. Evaporate nonpolar to yield fairly pure thc acid.

Im still learning but with your help i think im going by the correct direction to medicate myself, ive not said that ive making bho for three years and now everything perfectly, since i started to do i wished to know what nowadays im trying to learn but by this time i didn expect that could exist something purer than a good bho.

Thanks a lot for your help and time family. I appreciate it a lot.
 

99.99 thca

New member
Could pangea o weedalcoholic explain it carefully? Ive been reading everything for the last few months, in europe we cant have access to this medicine and i want to make my own, ive noticed that the only way to make it is with column chromatography or acid base extraction, once you have it for obtain the crystals you must use the crystallation technique.... This is very helpful but.... Could you guys explain properly again for the people that are studying the terms with this sustance? I dont know if its better to xtract bho from live resin and try to make a a/b extraction or with normal winterized oil is good to do it

Thanks a lot for this post guys ive been reading you for few months and the account was created for this reason, im an european patient that can have access to this, is not possible in europe, i only want to learn from you mates, this wonderful plant means a lot for me. Thanks for your compression boys

In tha last part i wanted to say that no one can have access to it and also i cant get it there, sorry for my english boys
 
@99.99Thca ..A/B extraction will work but may not be the most efficient. Chromatography is a way to produce THCA in larger amounts then is what is currently being produced. Some companies are selling the high cannabinoid fraction from their closed loop extraction as pure THCA, when it only tests at 80 percent cannabinoids, but of those cannabinoids present, 97% is THCA. This is a great starting point but not pure THCA by any means.

Slow-evaporative recrystallization would be the safest method to use. Follow Pangeas starting point of crystallizing from an underpurged mass of BHO. Clean and use these crystals to then experiment further(more recrystallization in different solvent systems) to obtain a higher purity.

Sorry for not posting more detail but there are many trying for this and until I can access the right materials, I dont want to show inferior methods and crystal. When I have enough to produce large crystals I will post further.
 

sadpanda

Member
hey guys im just wondering about the safety of smoking 100% thc? im no doctor but i ask because of 2 reasons, 1) we know how bad it can be to drink ~100% alcohol (but yes i know can't compare apples to oranges), and 2) last week i saw a video by a pro-cannabis & pro-smoker doctor giving a lecture at a uni in Israel. Anyway while she's pro-all-that, she is very concerned about DABBING ... but it wasn't made clear to me in the video if she was talking about how pure it is, or if its the effect of solvent residue, but she said it's the only time she'd ever seen toxicity in a cannabis patient.

Again im not a doctor and please dont be alarmed or anything, and again i dont even know if this is an issue or not, but its better to be AWARE than not, thats all!! so please make of it what you will :)

I refer to this - https://www.icmag.com/ic/showpost.php?p=7589928&postcount=5
 
A purified chemical shouldnt contain any residue solvent so that's not a worry. The concern would be people ingesting very high doses and getting increased side effects from that
Anecdotally, it appears generally safe at normally consumed doses. For very large doses, I think the jury is still out. As with any novel substance, start small and assess reactions accordingly.

She lost me at THCA dissolves in water, she doesn't appear to be fully informed about the subject matter. Her use of the word toxicity is ill advised. You see side effects yes, but toxicity I have yet to see anywhere in any journal or even personal experience.
 
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SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Smooth, comprehensive presentation on the current state of MMJ, unfortunately Deborah Kadabra doesn't want us dabbing her ass.

Thousands were dabbing on and on and on and on at Chalice California, check the records of the medical tent, no one falling ill as 'Debbie Downer Kadabra' would lead us to expect....... ;-))

She states most cannabis oils are devoid of terpenes, which we know is BS, and then she states the importance of titrating dosage, which we know is best achieved with highly concentrated medicine. A synonym for sanity is being reasonable....
 
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Pangea

Active member
Veteran
One year anniversary pics.

:woohoo:
 

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SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Thanks G.O. Joe... another conjecture to be disproved was raised recently, what happens when you put a liquid THC/THC-A solution in a centrifuge?

As to the wicked ass book I posted a scan from, I have nearly the entire book scanned and posted up at another forum, if anyone's interested I'd be glad to post it up here...

Cannabis related sections from the Psychedelic Guide to Preparation of the Eucharist,

http://www.tokecity.com/forums/show...rom-the-past&p=1316394&viewfull=1#post1316394

Derby this procedure is somewhat obsolete now, using a kromaton CPC machine is the way forward for prep scale isolates imo

How do you know it works? :)
 
Skyhigh - the thesis by Arno hazekamp titled "cannabis; extracting the medicine"

His paper covers cannabinoid isolation using CPC, proton NMR quantitative analysis, reverse phase hplc analysis, and thc complexing with beta-cyclodextrins
 

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