Hi,
I’m trying the exemple 15 of this SOP " US11352337B1 - Zeolite catalyst and method for preparation of aromatic tricyclic pyrans - Google Patents" but it’s not working, and this is putting me in a very shit situation, could anyone help me please…
I’m using zeolite linde type y, a synthetic form of zeolite, with a magnet stirrer, cbd isolate, and argon/co2 (ratio 80/20) gas to make it under vacuum (because I don’t have a pump yet).
I was putting 5.2g of cbd for 1g of zeolite, and the gaz, and then I placed my glass beaker (covered by an aluminium foil tightened with iron cable so that the gas didn’t escape) on the hot plate of the magnet stirrer when it was at 190°C.
Pls
Patents are NOT synonymous with SOP.
In fact they usually involve deliberate obsfucation of the required procedures and parameters designed to make repetition more difficult.
Eg: How are you adjusting the pH of your zeolite?
How does that compare to
The pH adjustment step may comprise contacting the zeolite catalyst and the base for a period of at least about 15 minutes, at least about 30 minutes, at least about 1 hour, at least about 1.5 hours, at least about 2 hours, at least about 2.5 hours, at least about 3 hours, at least about 3.5 hours, at least about 4 hours, at least about 4.5 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, or at least about 8 hours.
…and then you must dry it…but that patent makes certain not to tell you how long…
The pH adjustment step may further comprise drying the zeolite catalyst. The catalyst may be dried, for example, at a temperature of at least about 30° C., at least about 35° C., at least about 40° C., at least about 45° C., or at least about 50° C. The catalyst may be dried for a period of at least about 30 minutes, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, or at least about 12 hours or more. Optionally, the catalyst may be dried under a vacuum.
190C? How did you arrive on that temp?
An “SOP” would be explicit in both temp and time.
The patent? Deliberately written to leave you guessing…(preferably guessing wrong!…)
The conversion step may comprise heating the reaction mixture. For example, the reaction mixture may be heated to a temperature of at least about 70° C., at least about 80° C., at least about 90° C., at least about 100° C., at least about 110° C., at least about 120° C., or at least about 125° C. Typically, the conversion step is carried out at a temperature of from about 80° C. to about 200° C., for example, from about 100° C. to about 185° C., or from about 125° C. to about 175° C.
Are you using any sources other than that patent to guide your exploration?
Do you have analytics of any kind?
So what is happening to your 5g of CBD?
You might have the correct zeolite, or that might be a red herring thrown in to lead you down the wrong path…
You are not using argon to “make it under vacuum”, you are using it to “inert” the reaction; both are valid ways of removing O2 from the reactor, but conflating them implies a misinterpretation of this paragraph.
The conversion step may be carried out under ambient air. Alternatively, the conversion step may be carried out under an atmosphere comprised substantially of nitrogen. As a further alternative, the conversion step may be carried out under vacuum conditions.
…that you chose Ar/CO2 to inert with suggests a language barrier rather than simply missing the point.
The folks converting at scale are not using this method. Why have you chosen it?
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i think you’re better off abandoning this route.
patents don’t always (need to) tell the (whole) truth as @cyclopath said.
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