I’m a bit of a novice but would like to replicate what you did here. Any chance you’d provide a step by step with equipment? I understand the fundamentals but need a little advice on the actual steps. Would really appreciate it.
haha im not one to offer 
. Id recommend reading the experimentals listed in the paper above for a good starting point. If thats not self explanatory then you should consider studying org chemistry itself a little more.
12 Likes
Awesome advice @Benz3ne
3 Likes
I ran aqueous tosylic monohydrate with heptane in a reflux equipped spd boiling flask shielded with argon and got very possitive results. Difficult to do productuon this way but it worked.
4 Likes
You mean you ran a solution of PTSA in water with a solution of CBD in heptane?
What was end ratios of cannabinoids? Congrats
1 Like
I‘m really interesting! I‘m looking forward to your result!
maybe I have a Little tip for you:
Put toluene + (5-10%) and ptsa in the flask and make a destille setup. Now you destille the 5-10% toluene. Why? Toluene is able to make a azetrope with water, so its able to take the water from ptsa and when you destill toluene you have a higher boiling point as water have. So the first 5-10% which u will destill is toluene + water. Throw it away and in your Main flask there is anhydrous toluene and anhydrous ptsa. This Method works 100%.
But I‘m interesting in your way, too!
Or you take the ptsa in a vacum chamber, and heat up to 60-70*C (no idea if this work, I haven‘t tried)
Good Luck! And please write us your results!
Question: how do you get rid of toluene after reaction? Destill or purge? I think the problem is, when you destill without vacum thc oxidise to cbn.
3 Likes
Tolueen products have to be distilled
Ppm is to high yust purging
So is the scent treshhold
4 Likes
You could do it that way
1 Like
wish i got that with d9 
Simply heat it at 105c for few hours, and follow the mass loss.
4 Likes
That’s for cbd starting?
You just turn up the heat and you those times down by triple actually almost 5x
Ptsa absorbing water out of the air should not be causing you issues. It should only be exposed to open air for max 2-3 mins while you weigh it and should be kept stored in a sealed container. So idk how it would be pulling enough water out of the air to cause issues
I might be wrong, but I think Bhogi is referring to the monohydrate and is thinking that the anhydride would work better for his purposes
Higher heat will make the reaction go faster but it’ll also make more unknowns
1 Like
I think we were hoping you’d clarify about having used “aqueous“ tosylic monohydrate since many of us interpret that as a measurable quantity of water in your system, and we’re not sure it’s what you meant
I suspect the chemical dealer didn’t handle it adequately enough. I ordered a small amount of p-tsa from a small company.
I dried the p-TSA under vacuum with CaCl2 around it and was able to reduce weight by 3%
1 Like
330ppm of water is miscible in toluene. Therefore I don’t think that’ll get you the level of dryness we need. There are plenty of options for drying but I don’t think a dean stark trap is one of them.
Please correct me if I am wrong on that.
1 Like
No One really understands how to properly dry, many ways to skin the cat but only few can perfect the art of dry rxns. One day I may let out my exact sop beyond the few clients that have it but till then I’ll give helpful hints 
Happy hunting everyone
3 Likes