D8 Conversions, larger vessel ideas for process scale up

Hi all.

Trying to see if anyone has tips for larger vessels for conversions.

Exploring stainless options, I see there is mild corrosion experienced on the SS surface with PTSA in certain reaction situations.

Has anyone used true 316 stainless vessels with success for doing washing/conversions?

Ptsa and 316 do not mix from my understanding

Ion exchange will be the future of conversion

One column to do the reaction, another to neutralize the free hydrogens into water

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Wanna see if anyone has tried.

Most publication data I can find shows very low concentrations acrually cause nearly no damage to the stainless vessels.

Adding an oxidizing agent inhibits the corrosion factor entirely.

Anyone play with that yet?

You got anymore of those ion exchange links? Sounds kickin’ rad! I’ll be searching here as well, but damn that sounds cool.

Edit: I only see references to ion exchange for analytical chemistry.

Flow chemistry :grin:

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Never done for conversions but I have done a lot of ion chromatography for purification of virus. Used GE fineline columns for it. (Edit: anion exchange specifically)

Totally non related to cannabis: https://pubs.acs.org/doi/pdf/10.1021/jo01070a022

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How much larger are you trying to go? we need and idea on scale. Without reinventing the wheel you can easily do reactions in a 100L glass reactor. after you scale past that you can add another reactor.

there are benefits to running multiple reactors vs one. if something goes wrong in a 100l reactor you could lose that batch, or a good amount of it. if something goes wrong in a 500l batch well you lose 5x the product.

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Ive seen large glass lined reactors used for sale that are thousands of gallons, two stories tall and all. Im sure someone probably makes 200L glass reactors, but over that size Ive only seen glass lined stainless reactors

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We run 2) 100L glass reactors. We run the rxn in one then move the solution to the other for washing. The one we wash in has a filter on the bottom for efficiency.

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What are you trying to capture in the filter?

Anything that could have been in the isolate and missed when introduced into the vessel.

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Interested in the idea of ion exchange.

In aqueous this is done using loaded resins. What would you use as a donor/acceptor?

If you’re stuck in the mindset of batch chemistry you can get a used glass lined steel reactor as big as 1000 gallons. Otherwise, flow chemistry is the future of fine chemical manufacturing in general. Just depends what you’re capable of biting off.

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FTW @eyeworm