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Solvent recycling (mainly THF)

Started by jammin, June 24, 2004, 11:54:00 AM

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jammin

https://www.thevespiary.org/rhodium/Rhodium/chemistry/amphetamine.html



Is it possible to recycle thesolvents in this particular synth?

Im mainly thinking about the THF, but any info would be greatly appriciated.


eXcidium

That a good questions to ask, I wondered the same...

Tough if you managed to recycle it, you'll have to stabilize it with BHT (2,6-Bis(1,1-dimethylethyl)-4-methylphenol)

Cheers


eXcidium

Also, in the final step, it mentions :


The pooled organic extracts was dried over MgSO4, filtered and the solvent evaporated under vacuum.




Would someone be able to distill off the DCM, instead of evaporating it?

Thanks anyone




Rhodium

In regards to the recycling of THF, you might want to read this document:

Recovery of Tetrahydrofuran (THF)

(https://www.thevespiary.org/rhodium/Rhodium/pdf/thfrecovery.pdf)

You need to dry the THF fully, preferably by refluxing over sodium/benzophenone, but after the pre-drying outlined in the above document, it may be enough to reflux with molecular sieves or sodium/potassium hydroxide followed by distillation from a fresh batch of KOH/NaOH.

Would someone be able to distill off the DCM, instead of evaporating it?

Of course - distillation is evaporation, additionally followed by condensation of the vapors. From the perspective of the product it couldn't make less of a difference if the vapors was allowed to escape into the atmosphere, if they were condensed in a distillation reciever or even if you huffed them - it's all evaporation to begin with.