ILL NYE CBD-D8 Conversion Master SOP

Changes the pH of the aqueous layer? To see if a more vigorous stir drops out more SodiumBicarb and Salt? That’d be a good test, I’ll definitely try that out next run. :raised_hands:t4::ok_hand:t4:

Really? That’s super interesting. I’ll definitely run a few tests.

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What do you set your roto bath temperature to when recovering heptane?

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Just depends on your vacuum depth. I’m usually hovering around 60c.

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I will add Δ⁸ specific SOP’s in a few weeks. Roto, pretty hard to mess anything up there. Distillation… definitely some important parameters there. Just need to officially type up SOP’s for sort path and wiper.

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Nice. Yeah I’ve been recovering at 45-50c with a pretty good vacuumdepth on the 4c diaphragm pump and noticed my solution still a little bit runny when I pull it out of the roto.

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Nice those would be exciting to see!

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Yeah, like you stated… Roto is pretty self explanatory. But Δ⁸ distillation SOP’s are another crucial step of parameters. Plus, every damn short path or wiper setup is different. So specific parameters that work on my setup… may not exactly apply to yours. But there’s some good general “rules of thumb” ill throw into SOP format.

Easiest method:
Really really get your pH of your Δ⁸ crude dialed in. Then 2 steady passes on distillation and you should be water clear with no clays or scrubs needed.

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@iLLnyeTheShatterGuy does this rxn produce a product that is less than 0.3% D9?

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Will DM you :call_me_hand:t4:

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Yeah we talked on IG a little bit ago and I think we have similar set ups… I run the 2- 12l summit set ups laminar with the shorty fraction collector. I do also have a vta but I don’t run that for the rxns as I don’t know how it would differ from the SPD’s.

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Good morning :smiley: always nice to start the Future4200 day with a master piece !!:+1:
Personally your sop writing is 9/10 way better than my telegram / Morse code sop s

I would recomend writing CAS Numbers behind your reagents for it makes it clear as to wich version of the reagent you are using

Personally my recommendation is running the same sop at lower temps but higher stirring speed not sure if your reaction gives the famous red coloring so often seen with ptsa reactions
It was our grand master @Photon_noir that thought me this add acid while solution is around 25C and keep the temp below 35 C
While adding (exothermic spike +- 9C)
I run this rxn at 30C with a faster stirr 600 rpm
And my color of solution at the end of the rxn is amber
I also have noted that a rhigher stirspeed shortens the reflux time although I can not confirm if it spoils the yield Or not
Personally I prefure to filter out the ptsa prior to water washing it s a step that to. Me makes sense for I work on a stainless steel reactor and have to transfer my solution to glass sep funnel anyway
In my case this makes my reactor available for my next run
At last a small diffrance in sop is that once my solution is back to neutral PH 7 I pass it treu a bed of oven dried magnesium sulfate (2 hours in the oven at 250C) this rips most water out of the solution prior to distillation
I ll leave it to @Photon_noir to share the powder in the boiling flask to get brilliant water clear in the first pass :wink:
All in all you have done the community a great favor in sharing this masterpiece and I am humbled to be a part of it :clap::clap::clap::raised_hands:

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Thank you brother, that means a lot!

As always, I greatly appreciate all that you do for our community as well!

Wow, I absolutely see opportunity to change a few parameters you’ve mentioned and create a combined SOP. :call_me_hand:t4:

-Will increase stir speed on washes, take intermediates, and gather some data for us. @AlexSiegel also mentioned this and it’s clear that parameter needs adjustment in my current SOP. Thank you both!!

-Will absolutely pass through MgSO⁴ to help remove moisture. I believe residual moisture can cause unwanted reactions. Great advise, will definitely do that and gather data too. I initially was utilizing @Photon_noir amazing method for clay and color (It absolutely works). As I continued to work on pH neutrality by adjusting the NaHCO³/NaCl ratios during washes and tightened distillation parameters… I was able to conclude water clear without the need of clays (in most cases). Do you think passing warm Δ⁸ Crude:Heptane solution through MgSO⁴:Carbon or Carbon & Bentonite (to neutralize each others pH) would potentially pull unwanted pigments without having to do a full heated scrub or clay in flask? Would this potentially swing the pH in any way? I try to avoid clays and high heat resonance times as much as possible (too many pink and other hues looming around trying to ruin batches and pH). :expressionless:

Much appreciated brother :call_me_hand:t4::call_me_hand:t4:
#leveluptogether

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Now that is how an SOP is supposed to be written! GMP.

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Switch your lle wash steps around you won’t have as difficult of a time getting back to neutralization prior to distillation. We both of course know good parameters to distill D8 off at so I’ll leave it at that. But yes upping the Rpms on your seperation will allow for much better wash on the first go instead of needing to repeat steps. Also helps while letting sit to seperate to spin at 100rpms for 10-15 then 25rpm for 5 & finally sit.

Correct on the sulfate for removing moisture prior to distillation it would also help to pass through silica & 4a to remove more additional moisture prior to distillation. No one wants acidic/water compounds ruining a batch.

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Thank you brother, appreciate the kind words :call_me_hand:t4:

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Check “Wash Tips”

I’ll take a pH test strip on a small amount of the Δ⁸:Heptane solution after discarding the aqueous layer from each wash. This allows me to pivot accordingly before each wash. :call_me_hand:t4: My rule of thumb is… for every full point of pH, do 10 grams less of BiCarb or Salt depending, or do another distilled wash. Allows me to be dynamic as each batch is different.

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That wasnt my point…

You’re neutralizing out first with distilled water, which yes does work but will leave you with a little line of “foam like emulsion”, so I’ve found it much better & no need to repeat steps if you begin with bicarbonate as not only will it make the ptsa easier to remove from the organic layer but fully removes it if not filtered out like @Roguelab has advised.

I understand your point… it’s the exact same points that @Roguelab just pointed out in a previous comment.

ptsa finna become a controlled chemical like iodine

Good write up, thx for the knowledge lol

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Grab a Sigma account :call_me_hand:t4:

Thank you brother :raised_hands:t4:
Gang gang

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