CBD and CBG conversion to Delta 8 and 9

[Mosaic_Co-Labs]

While attempting to convert CBD and Delta 9 in hemp mother’s liquor to CBN I instead achieved a high efficiency conversion and isomerization to Delta 8 and Delta 9. I have attached the COAs from before and after and SOPs for everyone’s use. The parameters can be tweaked slightly to achieve complete conversion to Delta 9, isomerization to Delta 8 or degradation to CBN. Happy R&D gang!

Here is the summary of the conversion test we performed including equipment, procedures, and yields.

Materials used:

1.  SH-2 Stir Plate
   

2.  20mm flat magnetic stir bar
   

3.  Mercury Thermometer
   

4.  Infrared Heat Thermometer
   

5.  Stainless Steel Lab Spatula
   

6.  Gram Scale
   

7.  100ml Pyrex Beaker
   

8.  250ml Flat Bottom 24/40 Round Flask
   

9.  250ml 2-neck 24/40 Round Bottom Flask
   

10. Claisen adapter 24/40

11. 3-way Distillation adapter,75° 24/40

12. 2 x 24/40 Ground Glass Stoppers
    

13. 13.300MM Liebig condenser

14. Vacuum take-off adapter 24/40

15. 2 x Laboratory Stands

16. WVP-02 Water Aspirator Vacuum Pump

17. Circulating coolant bath -20C

18. Insulated Coolant hose

19. Vacuum hose

20. 2 Liter Vacuum Filtration Apparatus

21. Qualitative filters

22. C-Bleach

Procedures:

1.   110 ml of oil/pentane solution is taken from the mother liquor.
   

2.  Oil/pentane solution is added to the vacuum distillation apparatus and solvent is recovered yielding 51.52g of purged oil.
   

3.   14.61 grams of purged oil is added to a flat bottom 250ml round bottom flask and heated to 100C with magnetic stirring applied.
   

4.  4.61 grams of C-Bleach is added to the stirring hot oil.
   

5.  The material is brought up to 140C for 40min and 150C for 5 min with vigorous stirring to ensure aeration of the material.
   

6.  The hot plate is then turned off and the material is stirred until cool.
   

7.  The oil/c-bleach mixture is recovered with 99% isopropyl alcohol and filtered twice though double layered qualitative filters to remove spent catalyst.
   

8.  The isopropyl alcohol is then vacuum distilled out of the reacted oil mixture to produce a final yield of 10.0 grams (68% yield by wt.).
   

[Kingofthekush420]

This is why I dont use c bleach, you have alot of side isomerization guaranteed.

[Kingofthekush420]

Test for CBC, you have delta 10 in there guaranteed.

Which would show up as CBC

[anon93688]

CBD to d8 and d9 are known processes, CBD to CBN needs to be forced forwards.

[singlesource]

https://pubs.acs.org/doi/10.1021/acs.jnatprod.7b00946 other post on the site about this but I am going to be trying a slightly different method for the conversion.

[Mosaic_Co-Labs]

Yep. Just sharing my experience

[Mosaic_Co-Labs]

This was not from crude. It was mother’s liquor from hemp disty. Here’s the starting material COA from that distillate.

[Mosaic_Co-Labs]

These are the modifications that I suspect will achieve the following results. Please provide feedback!

-D8 from CBD and D9 = longer reaction, with same amount T-41 and No Oxygen

-CBN from CBD and D9 = Oxgen, higher temps and longer reaction/residence

-D9 from CBD = lower temps and lewis acid (H2SO4, HCL) with No Oygen

[Mosaic_Co-Labs]

Where can I get testing for CBC/D10? This lab, as you can see, does not have those standards. Also will D8 or CBC/D10 prevent recrystalization once reintroduced to high CBD disty?

[anon93688]

Lewis acids are electron acceptors…meaning that they have an empty orbital ready to receive electrons from a Lewis base.

Boron halides, aluminum halides, etc.

[Future]

@AlexSiegel for testing

[AlexSiegel]

Are you asking for testing of a material confirmed to have CBC and D10? We don’t actually have a method currently to deconvolute CBC and D10, one of the issues with testing in general.

[anon93688]

we should all pitch in to buy an NMR…that we can tell d10 and CBC apart.

[Mosaic_Co-Labs]

As I understand the presence of CBC/D10 in the material has not been confirmed. Please see attached COAs. I do not believe the lab had standards for D10 or CBC.

1. Distillate COA is after single pass distillation of hemp crude before crashing CBD.
2. Phase 1 COA is mother liquor after evaporation of pentane.
3. Phase 2 COA is after attempted conversion/isomerization outlined in first post on this thread.

[Kingofthekush420]

@AlexSiegel

Are you asking for testing of a material confirmed to have CBC and D10? We don’t actually have a method currently to deconvolute CBC and D10, one of the issues with testing in general.

I think he just wants to see if any CBC pops up, we dont care if its d10 or cbc we just want to see if it’s there and increasing in #s because if it is its d10 not cbc

[Dabatronicus]

I left that isomerized water clear From CBD I made open to air and am just letting it age to see how long it really takes to form CBN with just time and air.

Not super interesting but it’s easy to try

[phenethylamine1]

Here’s my general assessment of the experiment, based on the input/output weights and potency testing provided let me know what you think.

Input weight was 14.61g at 51.871% total cannabinoids which makes a total of 7.578g of cannabinoids on hand.

Output weight was 10.0g at 52.765% total cannabinoids which makes a total of 5.277g of cannabinoids on hand.

There was a 31.55% loss in total oil weight from the process.

There was a 30.36% loss in total cannabinoid weight from the process based off of test results and input/yield weights.

Based off the input/output weights and testing there was total gain of 0.602g 9THC, 3.200g 8THC, and .023g CBN on hand

Based off the input/output weights and testing there was a total loss of .129g CBDA, 5.047g CBD, and 0.950g CBG on hand

There was a compete isomerization of CBG producing a non-detect for the lab.

It seems to me that all the cannabinoids are accounted for when you consider the total process loss from material transfers, material absorption from the media, lost weight from decarboxylation of CBDA, and non-detect on modified CBG all accounted for in the data set provided.

I imagine there are still other trace side reactions that are not considered for in this data set because the lack of CBC, CBF, and CBE on the test panel, but I don’t see anything big that would indicate a large conversion to a unaccounted for Hydrocannabnol type isomer like a D10 or Cannabidiol type like 6CBD.

Based of the MSDS of the catalysist used the material “Natural bentonite, acid-leached and active carbon Bentonite”. The high heat, acidic solution, and exposure to oxygen is responsible for the almost complete loss of CBD from cyclization to THC and subsequent isomerization to delta 8 from the alkali bentonite clay. Total CBN on hand increased by 30% from the delta 9 THC exposure to air and heat, but most THC was locked in the delta 8 arrangement due to it’s higher stability preventing its aromatization to CBN.

If this experiment is attempted again I would recommend using even smaller equipment like a 100 or 50 ml flask and using quantitative filters so the amount of material absorbed by the c-bleach can be determined, but hey work with what ya got!

Carbon Chemistry T-41_GHS_SDS_5_18_2018(1).pdf (470.1 KB)

[Mosaic_Co-Labs]

Heard

[Mosaic_Co-Labs]

@phenethylamine1 Thanks for the insight! I’m going to DM you for a deeper dive if you don’t mind

[phenethylamine1]

hear from ya soon!