I agree with evaporating off your acetone and swapping solvents prior to water washing. That would work well as long as you use a hydrophobic solvent.
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I did for the isolate. Not the reaction. I’m distilling it now after isomerizing, and rewashing It via my traditional method.
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perfect tagline for @JedClampet Tek
“Nano Cowboy Tek”
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It’s common practice to use a saturated salt solution and a non polar solvent to take compounds
out of acetone and into a low dielectric solvent for water washing.
the idea is salting makes the aquas layer more ionic and pushes out non polar substances.
if this is the case for THC and CBD I am not sure but I would think it would be.
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If you only knew the clandestine stuff I do out here on the farm.
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Here’s a great primer on salting out (and salting in) that might get some here up to speed:
Turns out some salts are better for some things than others
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ye for instance calcium can play havoc on amines no end in fact a lot of transition element
salts and alkali earth (iron copper calcium lead list goes on) make amine complexes.
not relevant to cannabis but an example of what your talking about.
sodium chloride is safe in most instances.
great paper and great find Sid A+
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its not a good idea to use molecular sieves in the reaction mix with acids.
they are made with sodium or potassium ions depending on the angstrom size.
you will find that they just eat your acid and then become useless both in the reaction
and for drying when you try and regenerate them.
when using poly phosphoric acid I think you will find that the poly phosphoric acid will
dry your solution enough anyway.
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heptanes solubility in water is 0.0003% at 20C (Heptane - Wikipedia)
poly phosphoric acid reacts with water to create phosphoric acid.
H4P2O7 + H2O ⇌ 2H3PO4
so it takes about 1 mole of water to react with about 200g of polyphosphoric acid (it takes more
water than this but its a safe number to use in the case here).
poly is not always at the same level of hydration so it is impossible to get an exact number
unless one knows the level of dehydration the phosphoric acid has gone through so
I shall suggest that this figure is a good one to work with.
the recipe that uses 200g of polyphosphoric acid 1kg of CBD and 3Kg of heptane
should not have any more than 1 ml of water in it or 0.055 mole.
that means that 11grams of the 200 will be used to react with the 1 ml of water leaving
189 grams of poly phosphoric acid and 11 grams of phosphoric acid.
(edit that is wrong as the phosphoric acid gains weight on the polyphosphoric acid due
to its hydration but I don’t see the point in fixing it as it will make no difference to anyone
here just know I see the mistake 
)
as can be seen by adams ethanol isomerization to delta 9 phosphoric acid is a very good
catalyst for this so there is no problem with having this mix of poly and ortho phosphoric acid in the reaction.
I would personally say that unless you are extracting the CBD from an ethanol water solution
with heptane there is no reason to dry this mixture and the stoichiometry leads that way too.
on that line of thinking I would like to suggest a new catalyst.
boric anhydride (boron trioxide)
easily made from dehydrating boric acid in the microwave.
also reacts with water to create boric acid and dehydrate the solution.
enjoy.
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@squig Isn’t boric acid roach poison?
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boric acid softens the exoskeleton of many insects.
its salt is also used as a fabric softener for clothing.
hydrochloric acid and sulfuric acid are not nice but the thing about these acids
are that when they are neutralized with a base they do not dissolve in non polar solvents
like heptane and toluene.
borax is not much more toxic than table salt.
Borax, given the E number E285 , is used as a food additive
also on consultation with a friend on this boric acid can affect the stomach of some insects too.
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Boric acid is also very good for neutralizing HF.
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thankyou Doctor I love it when you check my posts
please keep doing so I often miss things
HF wow I had some ghetto boys give me 80 Liters of 40% hydrofluoric acid
thinking I could cook something with it.
after telling them that there was no way to stop it eating them if they got it on them
and that it could quite easily stop there heart when it hit there blood stream I ordered them
to return it to the factory they stole it from.
I think it was the first time I saw them shit scared hehehe.
there are some chemicals I am glad the public can not get.
oh myth busters used piranha or peroxide sulfuric for there pig test and
40% caustic at 60C+ is far better than piranha.
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delta 8 reference with 98% yield only one product measured vi nmr
https://future4200.com/uploads/short-url/i05lTYrFLQYNLIfNoBhOR0SKChP.pdf
you may need to extend the reflux time as they are dehydrating the alcohol
use toluene don’t bother trying to get benzene its carcinogenic
(though no where near as bad as the press will have you believe)
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a few ideas
Regeneration of a supported Nafion® catalyst for the double-bondisomerization of octadecenes
Regeneration of a supported Nafion® catalyst for the double-bondisomerization of octadecenes.pdf (1.2 MB)
https://www.sigmaaldrich.com/technical-documents/articles/chemfiles/polymer-bound-lewis.html
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Couldn’t one add water to the acetone solution and louche out the cannabinoids? I’ve done this with ethanol, can’t imagine why it wouldn’t work for acetone?
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references on converting delta 8 back to delta 9
Addition and Elimination of HCI to Tetrahydrocannabinol Isomers. A
Method for the Preparation of Stereospecifically 2H-Labeled Cannabinoids.
Addition and Elimination of HCI to Tetrahydrocannabinol Isomers…pdf (407.7 KB)
Novel Synthesis of trans delta 9 thc
Novel Synthesis of trans delta 9 thc.pdf (165.4 KB)
Umwandlung von ( -)-d6J-3, 4-trans-Tetrahydrocannabinol in ( -)-d’92-3,4-trans-Tetrahydrocannabinol
Synthese von Haschisch-Inhaltsstoffen
Synthese von Haschisch-Inhaltsstoffen.pdf (957.2 KB)
I wonder if there is another way to pull that chlorine off without a tertiary alkoxide
that will give delta 9.
this also brings up the question of adams isomerization with HCl in alcohol though he did
do it with 0.005% HCl.
it may be possible to use linalool instead of tertamyl which is cheap and available.
so the idea would be if you had a heap of delta 8 gas it in DCM too the chloro compound
then react that with potassium or sodium linalool alkoxide.
not sure if it would work but it fits the large tertiary alkoxide mold though it is unsaturated.
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The second paper is actually a synthesis of delta-9-11-THC from d8-THC with 9-α-Cl-HHC as an intermediate, This is another isomer.
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thanx what is the difference in activity.
the two isomers of Cl-HHC do they lead to different isomers of delta 9 ?
I know they purify the one isomer in the second via rp chromatography.
I have yet to translate the last two.
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