thankyou for sharing this 
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I am watching people do test runs in the 100 200 300 1000 gram range.
STOP IT
its stupid and waist full
why ?
get a small kit and do the reaction in the 5 gram range.
just because some dude wrote a SOP on something doesn’t mean it works even
patents and journals come up bunk at times.
every situation will be different your distillate solvent catalyst acid ect all different.
you have to tune this shit.
I am hearing of errors in SOPs that were sold ???
be wise test stuff on the small scale and then when you have results then step it up.
you don’t need a kilo to send it off to the lab.
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To be 100% honest I was disappointed with the results because I’ve be working for Non detect on the Delta 9 with no side reactions.
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understandable still but to find new information like what happens with citric in water
for isomerization is not a bad thing.
even our failures are successes if we gain information from it.
from what I can tell the route is CBD is turned into Delta 9 then the double bond moves
over to Delta 8.
maybe as suggested above its just a time thing.
use the optical rotation to follow the reaction next time you should see it move up to over 250 which is where you want it if things are going well.
it may be that at some point the rotation does not move anymore and then you know that the
path will not get to 100% delta 8 (if that’s possible)
but at least if your doing small reactions with optical rotation measurements you can do
lots of tests before having to send anything off to be analyzed
I still call it a success and thank you for the open sharing of information.
also for those going to CBN its great they don’t care if its delta 8 or 9 as they will
be dehydrogenating it anyway.
they want a food safe reaction and citric acid is used in food so there is a big win there
citric acid and water is pretty safe for human consumption.
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The citric acid was in tht case dissolved in the water. It is highly soluble in water. It buffers the solution to a low pH. The more concentrated it is, the more you will get close to pH 2.79, which is the pKa of citric acid.
Here you are limited to water boiling temp, unless you woulg go for pressurized reactor. You may just increase rate by playing with temperature and acid concentratrion, but not the yield. It may be only a question of time . If you want to check this well, you have to follow the reaction over time, and see what profile you get. From this you will be able to predict the trend over extended time, and thus the max expected yield.
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what about DMSO for the solvent ?
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Just curious, does this lab have ISO 17025 accreditation?
It’s the smallest equipment I have lol. Everything else is manufacturing/production sizes.
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I do need a way to follow that reaction over time. I feel that it could be dialed in very well. Only piece of equipment I have for analytics is a FTIR which I don’t believe will tell me concentrations. Should have never sold my Agilent 1200.
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How would you remove DMSO from the product?
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@squig is smarter than me. I had asked where to read about how to calculate how much acid is needed to catalyze a reaction. Without a Phd level understanding, the answer is optical rotation and testing small amounts with different variables.
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I’m confusing with another acid. 
The lowest pka is 3.13, so the lowest pH at high concentration will be about that.
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Shouldn’t these optical rotations have a couple more parameters quoted along with the value?
potential hydrogen is not the same as the negative log of the acid dissociation constant (Ka) .
pka works in all mediums its how easy the acid will give its proton and I hate the math behind it.
I had a tough job of doing poly protic acids in any media with pka
ph is the potential hydrogen in an aquas medium hence why we can not measure it in alcohol.
citric has three pka values one for each carboxyl group that can give a proton.
really im a shit chemist and a mediocre bee there is far better than me.
beaker was far better than I at these things.
nicodem at sciencemadness he is a true wizard and I would not be surprised if he works somewhere
like beayer.
im just board as im stuck at home on lockdown (again)
optical rotation can be measured with a protractor its just an angle to my knowledge.
having said all this if I even tried to pull the I know this shit on other forums I would be shot
down so quick its not funny because I don’t know it I kind of know it which is a big difference.
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again a heap of math and that’s just wiki
THC delta 9 is stated as −152° in wikipedia I think its a bit more of a span than an exact
number for most peoples measurements.
THC delta 8 from adams journal publication Isomerization of Cannabidiol to Tetrahydrocanabinols 1941 done with p toluenesulfonic acid isomerisation is stated at -264 to -270
when adams did his work there were no spectro gear like we have to day.
he didnt know THC 9 or THC 8 it was all recorded in optical rotation.
he even states Dependent upon the conditions used, the
tetrahydrocannabinol obtained had a specific rotation
which was reported as alpha D -160 ± 10" or
alpha D -240 ± 10". The results in preparing these
forms were variable. Even though carefully controlled,
successive experiments often gave products with different rotations.
he goes on to suggest a couple of reasons why it might happen either a double bond moving
or a change in levo dextro isomer so even with out the gear we have he was kind of onto
the reason for the change.
the paper can be found in AgTonik’s ref collection
there is a review of adams work that goes into some detail using NMR and IR and explains
the steric hinderence and why D8 is more favourable over time than D9
it is posted above as
THE ISOMERIZATION OF CANNABIDIOL TO TETRAHYDROCANNABINOLS Y. GAONI and R. MECHOULAM
it also has another hidden gem in it and that is cannabinoids precipitate with dinitrobenzoyl chloride.
a procedure is provided but here is a more general procedure for phenols
I think you get funky colours too (notice the english colour there) so it may be that
CBD and THC have a different shade or colour to them.
also being the CBD has two phenolic groups it may again have different solubility properties
allowing for separation as the ester and then hydrolysis back to the CBD or THC.
also may be a cool way to drop cannabinoids (with the phenols of course) out of crude
Compound Via (250 mg) was warmed at 70” with 3.5 dinitrobenzoyl chloride (400 mg) for 4 hr
without a solvent. Benzene (20 ml) was then added and the insoluble dinitrobenzoic acid was filtered
off. The solution was washed with 5 % NaHCO,aq and water, then dried over Na,SO,. The residue
obtained upon removal of the solvent was chromatographed on 50 g silica gel and eluted with pentane-
ether 97 : 3. The dinitrobenzoate obtained was recrystallized twice from pentane, giving crystals
m.p. 125-127”. (Found: C, 65.77; H, 6.65; N, 5.79. C&HI,NIO, requires: C, 65.87; H, 6.71;
maybe a way to extract OTC CBD mixes which will be all we will be able to get in time
due to this thread
no you can not patent it I will prove it was not yours as we all can now.
I forgot to mention its recrystallizable and due to it being an ester and more polar now
might happily go through normal phase chromatography to separate the cannabinoids.
purification to the max
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Who on here is conducting cyclization test runs with 100g or more?
What I was getting at is for each of those measured optical rotations a temperature, solvent, light source, path length, and concentration were mentioned. From this measured rotation the specific rotation was calculated.
ethanol no temps on wiki temp vary around mid 20’s to low 30’s in adam’s work but show similar
rotation hence the range rather than a solid number.
sorry miss understood you
Will this affect the lewis acid reaction? 4a Molecular sieve beads remove water. I was told to only use the beads for conversion to D9. Could be wrong, any insight will help.
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