Hello everyone,
I'm following a protocol in which 1 ml of diethyl ether is used as a triturating solvent. The product should remain a solid while the impurities should dissolve in the diethyl ether. I'm then supposed to filtrate the solution, however diethyl ether is very volatile. If I use vacuum filtration, the diethyl ether will just evaporate immediately leaving my impurities with my product. But if I use normal filtration, I expect the diethyl ether to also evaporate long before passing through the filter.
What approach would be best for this? I'm thinking of either doing a normal filtration where I keep dripping fresh diethyl ether on top to prevent if from evaporating dry. My other idea is to instead of pulling a vacuum below the filter, to have air pressure push the solvent through the filter. (maybe even elevating the boiling point a bit)
For those who want to see the protocol, it’s DASA-5 on page 8 in the supplementary document from the paper: "Promoting the Furan Ring-Opening Reaction to Access New Donor– Acceptor Stenhouse Adducts with Hexafluoroisopropanol"
Thanks in advance!
Have you tried using Buchner filtration? Also, your product is insoluble in diethyl ether right?
To clarify, by vacuum filtration I meant to say buchner filtration. The product should indeed be insoluble in diethyl ether.
You can try another solvent for Solidification.
Like mtbe ether, Diisoprpyl ether. Pet ether.
Ashok Kadam Thanks for the suggestion, by now I've been able to precipitate my product in a different manner. By combining recrystallisation techniques with diethyl ether as an antisolvent, I was able te get some product. This question can be considered solved.
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