Experiment results, CBD->THC using, DCM timings + chromatograms only :)

[xdubr]

I have had my previous DCM,pTSA experiment.
It was 90 minutes 50/50 isomers with 2% cbd left.
I just wanted to get into the details - and as i do have my own chromatography machine to play with - it will be a lot of pics.

Last time in 90 minutes, DCM (2:1 ratio) , PTSA - I got my first ever conversion. I got nice twin-peaks of the isomers - and I wanted to see for myself how it ended up there. And as I happen to have an HPLC UV to play, I wanted to see how it got there.

(Warning, lots of pics) :

DCM:

CAS: 75-09-2

Molar mass: 84.93 g/mol

Water content: 0.02%

Producer: Thomas Baker

pTSA:

CAS: 6192-52-5
Molar Mass: 190.22 g/mol
Producer: Sigma-Aldrich™

CBD:

CAS Number: 13956-29-1

Molar Mass: 314.46 g/mol

Producer: —

100ml DCM : 50gr CBD Ratio

0.5gr (1% PTSA)

Timings: diluting 0.5 ml to 25ml methanol - test ph and analyse.
Methodology:

100ml dry DCM : 50gr CBD (2:1 ratio)
1% (0.5gr pTSA)
RT (21)

Last time it was 90 minutes 50/50 isomers with 2% cbd left. So

Took a sample of 1 couple drops every 15 minutes, and starting specs:
Column 150*4.6

Test timings(mins) : 0,15,30,45,60,75,95. Cause of DF - last 2 chromos extended to 10 mins.

![IMG_9252|690x319]

(upload://wnLO88YEfvB0F5D5gkQlsuQpkCv.jpeg)

[Math]

how to read the data? How many % of d9 and D8 did you get?

[xdubr]

Thank’s for a question. So the results were as follows

Minute: CBD, d9, d8

Minute	CBD	Δ9 THC	Δ8 THC
0	98,513%	0%	0%
15	57,240%	39,056%	1,563%
30	38,807%	47,258%	11,124%
45	14,078%	40,468%	41,408%
60	0,613%	43,713%	50,709%

Then the d9 starts slowly fading away (sorry, the picture of the results is somewhat blurry, but i reckon it was ND/30/60 at the end of the run.

[kcalabs]

We learned so much running the reaction ourselves years ago. We also sampled early and often.

As mentioned, you see D9 is the first product and then D8.

On a parallel pathway you’re creating D8-iso-THC and then D4,8-iso-THC, which are both coeluting with the D8-THC and D9-THC, respectively.

[Math]

thank’s