We are dealing with something small here, I don’t think it’s much larger that the little hump at 6.5. And it is clearly not d9 from here.
And you clearly see all the other peaks in the overlay are very nice. But not the isolated d8. I bet there is some of the intermediate/competitor that is in all synthesis (but to various extent, from trace to 30%).
anyone see this yet?
its not solvent as such but the ability of the solvent to dissociate ions would me be my thought
hence the acetic acid but …
ethylacetate is quite polar as well.
as we both know molecular collisions is important
but
we are dealing with electron movement from either an electron accepting species ie lewis
or a proton giving species ie bronsted
so to further accelerate this solvent could have a influence if it is ionic as both of these
reactions are ionic (I know dielectroc is old as dudes but im still counting reductions as nascent hydrogen)
my thought is that solvent is everything to do with it.
I am happy to be wrong but
they and there is many to the voice of they that water makes D8 quicker (I do believe that some have
it down)
water is very polar and helps in the dissociation of ions or the transfer of electrons and protons.
so why not just use a more polar solvent ?
ethyl acetate is a very interesting idea
as is DMSO but not for HCl as it helps to hyrochorinate alkenes in a big way ie huge side reactions.
I think I posted that in my journal thread
dont rely on cops for chem they often publish bullshit to get convictions
mother …s
3D Printed Polarimeter
https://pubs.acs.org/doi/pdf/10.1021/acs.jchemed.9b01083
A high-resolution polarimeter formed from inexpensive optical parts
A high-resolution polarimeter formed from inexpensive optical parts.pdf (2.6 MB)
“A polarimeter can be constructed using a document camera as a visualizer and a standard smartphone screen as a source of polarized light. A pair of 3D glasses can be used as a polarizing filter, and the optical rotation angle of liquids can be measured using any free compass app. Consequently, a demonstration of optical rotation can be conducted with no preparation time or specialized equipment.”
ive used this for checking glassware, except with just plain polarized sunglasses and smartphone.
https://pubs.acs.org/doi/10.1021/acs.jchemed.7b00767
Havent tried it for anything else yet, and dont have any 3d glasses laying around, but gonna order some now LOL
I think we need to get a working procedure for cheap following of optical rotation dur in isomerization.
its just too costly to continually send stuff for testing and at least with optical rotation we can see
if we have moved any closer to our target before paying out more money.
as far as the hardware goes, the paper I posted above claims build cost less than $400. Heres the supplementary info with the parts list and annotated pictures. https://static-content.springer.com/esm/art%3A10.1038%2Fs41598-020-61715-7/MediaObjects/41598_2020_61715_MOESM1_ESM.pdf
Call me a Philistine gentlemen but could someone clue me in on how I can use measurements of optical rotation to evaluate reaction completion? I don’t have much classical chemistry training so maybe I missed this one. I understand exactly how to build that piece of equipment but can I really use it to establish a d8:d9 ratio? Cause that would be sweet!
Thank you for breaking this down for me!
3g of CBD
100ml Isopropyl Alcohol
1gram of table salt
4 drops of 98% sulfuric acid.
2 hours maybe longer needed good stoning high so good D9.
Sid you need to extract some of the reaction mix and then maybe strip off the solvent
1 gram of sample should be put to 100ml of ethanol.
take reading of alcoholic solution in device.
-130 degrees is THC D9 plus or minus a bit.
-260 degrees is THC D8 plus or minus a bit
the measurement you get from the polarimeter will tell you which one you are closer too as
if you have more D9 you will get a number closer to -130
if you have more D8 you will get a number closer to -260
3g of CBD
100ml Isopropyl Alcohol
1gram of table salt
4 drops of 98% sulfuric acid.
table salt is put in flask with alcohol then the sulfuric acid is dripped in and flask swirled to mix.
flask was then heated to a boil and when boiling CBD is added and
condenser is placed on top of flask.
solution was refluxed unstired for exactly 2 hours.
when 2 hours was up I poured the mixture into 400ml of cold water and then extracted
with 70ml heptane
then again with 30ml heptane.
both heptane extracts where put together and shaken with 200ml of saturated bicarb solution
and then with plain tap water.
heptane was removed at atmospheric pressure I did not use any inert gas beds or protection
there where traces of water still in my ipa
there is more salt than h2so4 so you will get a nice moon rock of na2so4 with some skittles of
crystal salt to prove you didn’t add to much sulfuric 
pay attention to bring to temp before adding CBD.
I am making HCl in a measured amount from the table salt and sulfuric acid insitue.
I want it converted before I add my CBD.
I also want to know the time of the reaction rather than how long it took for it to start and then how
long it ran.
that start is an unknown as your conditions are changing.
then I dump it into cold water.
done reaction finished when I choose not when the environment around me the thickness of my
flask how cold my fridge is etc.
its diluted and cold now so no more reacting.
I have control of the exact start of reaction and then the exact end.
now I can start playing with ratios as I have a way to measure reaction time.
I will write this up properly soon when I get some analysis on it.
It wont be pure delta 9 no way but its clean and quite strong.
much much stronger than the phosphoric acid alcohol isomerization in adams 1940’s paper.
from what I have read it is to be expected in the 50% 60% range.
the oil was so near clear it was not funny. 1 gram stayed an oil after being left in an open bowl
for two days.
it was possible to smoke and vape it without distillation without bad taste or discomfort.
better than the phosphoric acid one which made me cough non stop.
I wonder what the change in yield would be if I where to use dioxane instead of an alcohol
or an alkane for my solvent.
nice ether with a 100C boiling point so I think its going react it a little quicker I think as we get
a halving in reaction time ruffly per 10C higher we go and a doubling for every 10C lower we go.
should turn the reaction into a 30 minute one.
dioxane is piss easy to make and slightly toxic 
though it is soluble in water so making my quenching technique possible.
If it works I will not be writing it up.
oh the doubling and halving of reaction time is dependent of hitting a reaction activation energy
state.
ie there is in some cases simply a temperature to low for the reaction to work at all.
shameless plug.
all experiments were done with jed clampet CBD.
https://future4200.com/u/jedclampet
his product is very pure.
I can not guarantee that other sources or extracts will have the same
results unless they have the same purity.
I could not have done any of these experiments with out his endorsement.
Hmm, I think I now know who to thank for bringing us @squig lol
there are many others who have helped me in this case it was jeds contribution that made it possible.
Hi all! New to the forum, and somewhat new to the cannabis industry. I am a professionally trained chemist/materials scientist, so I know a couple things, but I acknowledge I have lots to learn.
Anyway, I have been able to get 96.5% d8 and 2.4% d9 from CBD isolate. I am using pTSA. Can anyone recommend a means to get less than 0.3% d9?
No way you’re getting that from pTSA. I think this post is a ruse. Just me two cents
With the right procedure his results are definitely possible.
next batch …
same ratios and reaction time and temp ± 4C but instead of extracting with a cyclohexane heptane mixture I used xylene and used 95% ethanol in the reaction instead of IPA to test the water changing
the ratio of D8 and D9.
I can say that it looks like it makes a big big difference though I need to run a wet IPA to make
sure.
this product is no where near as strong as the one I got before and the consitentcy is a lot
thicker than the ipa reaction.
also the product went red after evaporation of extract solvent if that is due to a ketone in the
denatured alcohol or interaction of the solvent I am not sure but I am leaning towards
the xylene being the cause as the reaction was clear and the extraction a very light yellow.
so from this experiment I can say that I believe that Future4200 rogue’s advice
that water makes a big difference is 100% true.
I think drying the IPA should be tested now and for the reaction after an inert gas bed to see
if taking oxygen out of the equation makes a difference and then finally I think n-butanol would
be an idea to see if higher temperature makes for a better reaction.
I think keeping the reaction time the same is important as we are then testing each individual change
(yes I changed more than one thing this time water and alcohol but lockdown cant get ipa)
I would be supprised if drying IPA makes a big diffrence from undried IPA as
IPA is pretty dry normally as it is but ill test it anyway.
of course I should take the drying agent out before reacting.
the product is still smoother to smoke than the alcoholic phosphoric acid reaction.
I guess I could also put the strength down to the temperature difference of 4C meaning I should
have maybe put another hour onto the reaction time.
though the parameters are closer to what adams did this way except for the 5% water.
after a little thought on the colour change it may be due to the bicarb reacting with the phenol
in the first wash and some of it staying attached to the phenol when I stripped the solvent off
xylene is a wet beast compared to heptane and might have carried the ion through water wash.
so I could then put the thickness of oil too unreacted CBD rather than over isomerized delta 9.
the oil is also kind of skinning like it wants to crystalize so I would say that the reaction was
far from complete.
Are you able to have that properly tested where you’re at?