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Author: Subject: CBD oil extraction then conversion to Delta-8
organicchemist25
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[*] posted on 31-3-2021 at 19:24
CBD oil extraction then conversion to Delta-8


Its been a while since I have posted. I started a hemp farm last year and 2021 is the start of my second year.

I sold a good amount of my CBD flower from 2020, but still around 600 pounds left. The new thing is Delta-8 THC.

My questions are can anyone give me some experience and tips on extraction the CBD, then coverting it to Delta-8 and then separating the components.

So, for now, I am going to grind up my buds and just put enough N-Hexane in to cover the top of the flower. This will be done in a 5 Liter, 2 neck flask. I a going to reflux. The time is still in question. I will try a few different intervals.

Then I will evaporate the hexane it the rotovape to retrieve most of my solvent back and isolate the extracted CBD and Im sure among other things.

The next thing is to separate the CBD for its constituents that were extracted. I am thinking liquid chromatography with a little bit of positive pressure applied. The pressure is still to be experimented with.

Once the CBD is isolated I would like to make CBD isolate crystals. That is still in need of some research. I am not finding much of any direct literature on this.

I am going to react the CBD in a Lewis acid and organic solvent. p-toluenesulfomic acid in toluene. If there are other routes, please share them if you all would. That would be greatly appreciated.

Can anyone help with eluting either the CBD on first separation and then delta-8 etc. That is my weakest point; liquid chromatography. Really all chromatography. We only did one thin layer in Ochem and that was 6 years ago. I have columns and understand completely about packing it, setting it up with solvent, sand, cotton at the bottom and never allowing the solvent to drop below the top layer. Also, I do have elutent that is kind of old. Its silica. Not sure on anything else at this point. I rememeber there were a few choices when I bought it. I never got around to use it.

I have read about spot testing on thin layer or HPLC. Would I need HPLC, or for small scale at first use thin layer and liquid chromatography until I see if I am getting enough out to buy bigger, more expensive industrial equipment.

So, possibly in a nutshell, how would one go through the motions of this to reach the end goal of Delta-8?

I think there will be a few components to separate. Even some THC-9. How will I know how to identify each component? They may not have colors.

So the main issue I am the least educated on is chromatography.

How to isolate my CBD in step 1 and then how to isolate the Delta-8 after I react the CBD. I feel both will require chromatography. There will be other components in both steps. I just would like to gain as much info on that aspect as possible.

Thank you for any and all detailed help! Ive learned so much off this site.



[Edited on 1-4-2021 by organicchemist25]

[Edited on 1-4-2021 by organicchemist25]
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zed
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[*] posted on 31-3-2021 at 23:20


A couple of links would be nice. It is a complicated question, and you are making us look everything up.
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OldNubbins
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[*] posted on 31-3-2021 at 23:27


From future4200.com
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zed
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[*] posted on 31-3-2021 at 23:54


Chromatography? I wouldn't.

Vacuum distillation? Yeah. Maybe short-path.

Legal in my State. Well, quasi-legal. Can't do it in my neighborhood though.

Too many houses have been blown-up.

Such activities are restricted to commercial/industrial properties.
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draculic acid69
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[*] posted on 1-4-2021 at 00:29


I'd recommend making a tea with 1gram of it. I "heard" it is delicious as a green tea substitute. Would Highly recommend. Theres a large and growing market for hemp tea
regardless of thc/CBD content.
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organicchemist25
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[*] posted on 1-4-2021 at 10:02


Quote: Originally posted by zed  
A couple of links would be nice. It is a complicated question, and you are making us look everything up.


Sorry I didn't attach any links. Mainly stuff I found was YouTube videos and info sites just explaining the process. more for advertising their capabilities and contact info.

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organicchemist25
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[*] posted on 1-4-2021 at 10:12


Quote: Originally posted by zed  
Chromatography? I wouldn't.

Vacuum distillation? Yeah. Maybe short-path.

Legal in my State. Well, quasi-legal. Can't do it in my neighborhood though.

Too many houses have been blown-up.

Such activities are restricted to commercial/industrial properties.


I definitely didn't mean to come off as making anyone look things up. I was just thinking the more experienced people would just kinda know the motions of extraction the oils then the chemistry behind separating them further individually.

I go vacuum distillations often. I have a pump that easily pulls .001 torr/mmHg

I don't know why I didn't really think of that. I all kinds of condensers and lengths, but not a short path. I have a pigtail to collect fractions too. Ill order a short path. Im sure I can find literature on their boiling points. Im sure they may be fairly close in temps, so I will fractionallly distill if needed.

thank you for the help. You definitely pushed me into the right direction.
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organicchemist25
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[*] posted on 1-4-2021 at 10:14


Quote: Originally posted by draculic acid69  
I'd recommend making a tea with 1gram of it. I "heard" it is delicious as a green tea substitute. Would Highly recommend. Theres a large and growing market for hemp tea
regardless of thc/CBD content.


Ill have to give this a try! Thanks
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organicchemist25
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[*] posted on 1-4-2021 at 10:17


Quote: Originally posted by zed  
Chromatography? I wouldn't.

Vacuum distillation? Yeah. Maybe short-path.

Legal in my State. Well, quasi-legal. Can't do it in my neighborhood though.

Too many houses have been blown-up.

Such activities are restricted to commercial/industrial properties.


I am definitely not performing this at home. I am licensed and its on 15 acres inside one of my warehouses with 20 foot ceilings, concrete floors and walls, and ventilation. I am just interested in doing the chemistry myself rather than paying out a lot to get it extracted and processed with other companies.
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karlosĀ³
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[*] posted on 1-4-2021 at 10:34


I do that regularly.
By "that", I mean, the acid catalysed ring formation on bought CBD of standard commercial quality.

Over the course of that, besides finding the most attractice route for the delta-9 enantiomer on accident too, I even became pretty fond of the only half as potent, while causing less undesired side effects(e.g. mainly confusion, which rarely can turn into full blown paranoia).
Opposed to plant derived cannabinoids(=weed of course), I never get that with the semisynthetical delta-8 THC!

And of course, its also a matter of time... a yield of 90% is always ideal, but if you obtain that much after just an hour of refluxing with tosic acid in toluene, or if its leaving almost the similarly composed reaction, with the same yield expectations quantitative, but for 48h instead...?
In turn resulting in the only twice as potent delta-9, while requiring only 1/48th's of thats reaction time, but sadly resulting in the delta-8 instead.

Its simple math actually :o
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[*] posted on 1-4-2021 at 13:21


Quote: Originally posted by organicchemist25  
I am licensed and its on 15 acres inside one of my warehouses with 20 foot ceilings, concrete floors and walls, and ventilation. I am just interested in doing the chemistry myself rather than paying out a lot to get it extracted and processed with other companies.


Any unmentioned foreign substances?

Hire someone who doesn't need help. You don't know what to do, so you and google want us to say how to make a q-mill (assuming 10%, $10/g - costs) by mixing chemicals together for people to ingest...do you also want your OTC and prescription drugs made this way.




"You're going to be all right, kid...Everything's under control." Yossarian, to Snowden
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zed
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[*] posted on 1-4-2021 at 16:42


Well, it is something I have considered. The pot people, are following no rules and are not subject to inspections. Mostly, they aren't chemists, and there is no knowing what residues might be present in their products. Unless of course, the game has changed during the last few years.

I used to know a producer, who would call me occasionally for direction. My advice was usually simple.
Use hot ethanol. Use the good stuff. Beverage grade. Recycle it.
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[*] posted on 1-4-2021 at 17:10


Your proposals are awfully vague.

It reads like you spent about 10 minutes researching this, and have very little knowledge of purification practice.



Are you still trying to make ketamine too?
That was the last project you were asking about.

Well, I suppose with all those concrete walled warehouses with 20 foot ceilings you have plenty of room for all these projects.















They always say, "He lost his battle with cancer." But as Norm MacDonald pointed out, the cancer dies at pretty much the same time you do, so doesn't that make it a tie?


















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