I agree, I too was surprised to see that this wasn’t the case and posted it up. We can’t always only care about the chemists already doing theses methods, IMO. Gotta help those trying to learn as well. 
NDT Δ⁸ is also much harder than others are accepting or admitting. Again, another reason for posting this SOP. Every Chad I see believes they have NDT Δ⁸ like they purchased it from Cannabis Jesus himself.
This SOP is to help those who want to make THC and don’t know clear methods yet, other chemists to break apart my SOP so I can learn and better my methods, and just as a base of general knowledge for the squad. The more we’re transparent about our methods… the closer to NDT we’ll get. If you have any tips to help those get closer to NDT… please post them (if you haven’t already, not sure what’ve you’ve posted up). 
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Can toluene be replaced with something like naphtha or dme?
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Heptane preferably if changing solvent.
Keep in mind to degass solvent prior to homogenizing.
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What you need for ND D9 is a diffrent sulfonate acid and a solvent few people like
Wich is DCM
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Preparation steps for
CBD- Δ8THC via PTSA
(Always use proper PPE & safety precautions while undergoing any of these procedures for your safety & those around you.)
Preparation of degassing solvent
- Using a 5-20L bottle neck style with a inert gas/ vacuum adapter (inlet with minimum 175mm down stem & outlet GL style fitting rated for solvent.)
- Fill bottle neck vessel 3/4 way full with solvent of choice (toluene or heptane.)
- Begin to percolate flow of argon or n2 (preferably argon) at 15-20psi on the regulator for minimum 45minutes to a hour for up to 3-5L batches, more volume will require more time for percolation. (Subsided bubbling will occur within solvent from percolation please for your safety do these procedure in designated fume hood with ventilation out of immediate vicinity.)
- Once time has elapsed stop flow of inert gas percolation & remove solvent to storage container filled with dessicant( 4a beads) till ready for use. If ready to homogenize to oil, then of course proceed & add to vessel for reaction.
Adding solution to reactor or
short path
- This should be done under vacuum or with inert push & schlenk line on short path or multiple inlet adapters staged on reactor lid) after sparging the vessel 3 times at 20 psi then adding solution to vessel.
- Continue sparging after added & while at 550-600rpm (in reactor) 1200rpm (short path.)
- Release atmospheric pressure from vessel & use funnel to (as fast as possible to avoid atmosphere into vessel) add ptsa mono hydrate to vessel.
- Reseal vessel & continue flow of inert gas ensuring to use a oil/water bubbler to gauge atmosphere leaving vessel. (Depending on either fritted down stem or open you should be seeing 3-5 bubbles every few seconds with open & fritted you’ll need to ensure you’re not over percolating the bubbler as it will begin to build volume within the bubbler & overflow.)
Preparing PTSA
- Open sealed container from dry dark storage & use freshly cleaned & dried utensil to add to beaker & backfill with inert gas as to keep atmosphere from ptsa so it doesn’t retain moisture & “brown out”, then cover with press & seal till ready to use. (Preferably Mill down the ptsa with mortar pestle then add to beaker after weighing etc.)
- Reseal container of ptsa with adequate seal or lid & it is optional to backfill container with inert gas to keep atmosphere from entering ( will need a tight seal.)
- Return to storage till ready for prepping again.
- If moisture is present in ptsa you may try a desiccator to remove moisture or flame drying the ptsa under vacuum. (Use extreme caution when using open flames in lab procedures.)
Prepping inert gas regulator
- Place inert gas tank equipped with proper regulator for tank valve, ensure it is properly sealed before proceeding by bleeding open through regulator for brief moment to check seal(s) on regulator. (Make sure regulator is fully closed before bleeding as to not cause alarm to yourself or others by blast of gas without notice.)
- Once seals are checked & good to go, open tank with regulator closed.
- Add tubing from regulator to gas inlet adapter/schlenk line ( for short path) or a vacuum/inert gas adapter for reactor lid.
- Once connected continue direction of flow for vessel (short path through top of vertical condenser) or (reactor through outlet vacuum port for condenser) & add tubing to connect oil/water bubbler setup.(preferably t joint off the outlet of bubbler & line out to ventilation to remove gasses/vapors from vicinity.)
- Once thoroughly connected & setup, check flow & seals of joints while under inert gas flow to ensure vessel is sealed & scarfed of atmosphere. (Sparge at 15-20psi slowly bleeding in as to not blow a joint out of its place.)
Preparation of LLE bases & washes
(Use distilled water for all wash solutions)
- Prepare 1:1 volume of reaction solution : wash solution for washes on each step.
- Use distilled water to dilute sodium bicarbonate & obtain a ph of 9 with consistent ph monitor active while homogenizing base solution. (SODIUM CARBONATE allows for ph of 12 if wanted.)
- (OPTIONAL) use distilled water to dilute citric acid into solution with ph of 3-4 & use this base wash for LLE inbetween bicarbonate & saline base washes to remove any unwanted solubles in that ph range.
- Once homogenized & solution isn’t over saturated with bicarbonate stage as step 1 of LLE close by to vessel for LLE (reactor or sep funnel.)
- Use distilled water & 5% salt to create a saline solution, homogenize together & stage as step 2 for LLE.
- Use distilled water with a ph of 6.5-7 to stage as final wash for LLE & make sure to test ph of aqueous layer upon removal to ensure ph of organic layer is at same ph of water before adding to last wash for LLE.
- If using short path you’ll need to add oil from short path boiling flask to first base wash of LLE in sep funnel or reactor. (Optional to filter ptsa out prior to LLE to make washes easier.) If using a reactor, either add washes for LLE via vacuum inlet with tubing to solution or through a inert push into reactor.
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Nice additions and clarifications.
Also hate to beat a dead horse but I pretty much read entire thread just now, and is heptane really that hard to dry? I’ve always stored it overnight under Mg/Na S04 and never ever had any issues, though I’ve never used it in anhydrous reactions…
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Thank you!
Dessicating overnight is always a sure way to go, but bot always the quickest & it’s much easier to azetrope the toluene as described above. I used to use heptane but never got as clean of a conversion with minimal isomers.
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I have a hypothesis that since d8 is more stable than d9 due to steric reasons, the stiffer more electron dense toluene increases the free energy difference between d8 and d9 pushing equilibrium more to d8. Floppy solvent molecules like heptane have the opposite effect. Not a computational chemist at all so cant actually test this at all.
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So once Distilled through a short path are you clear of residual solvents?
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Correct, & if unsure of residuals coming out of roto prior to spd crank spd temp to 110-115 & pull the rest off for 15 minutes prior to increasing temp. It’ll all go to the cold trap anyways if done properly.
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@GroovyOctopusLabs
Short path when distilling off cannabinoids
At temps around 180C and hard vacuum
Is as if we are boiling at 400 C at normal atmosphere pretty sure all solvents are gone 
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Well I mean when I saw the word toluene I was like " 
"… Just wanted to ask.
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No I hear that & it’s completely understandable, it’s just a matter of the technicians capability IMO if they can’t or don’t fully remove residuals from any run.
It’s like moonshine, gotta cut ya heads.
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Then you have placed the A back and would be a fool to heat it up again
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yes, I have used a similar solvent mixture (hex/acetone 80:20)
for years…developing only 8 cm or so for rapid analysis.
I have seen similar conversions when using HCl/aqueous
as an acidifying agent. Amazing how fast things rearrange.
But not so with concentrated AcOH…nothing.
With regards to the TLC…I do not think a lot of people
realize how you can "mock up"a flash column separation very quickly
using TLC…then tweek solvent selection for best separation…
or quick qualitative analysis of various liquid-liquid , liquid-solid batch
separation systems .
Look at chromatograph #3 in fig. 5 in this blurb by Waters.
https://www.waters.com/nextgen/us/en/library/application-notes/2016/separation-thc-enantiomers-using-trefoil-chiral-columns.html
this is CBD to d9 using HCL in ethanol.
if you don’t want d9…keep the HCL in the storage closet. I imagine the phosphoric acid conversion noted above is similar.
btw I’m not interested in the conversion of CBD to anything…
it was a problem I was dealing with: extracting with water/high pH/reacidification…for those that know what I mean.
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I tried this for shits and giggles an there was still like 3% d9 according to kca.
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At what temp cold is what you need to run
