Useful experimental method for removing solvent #memo #organic_synthesis

There are many kinds of solvents are used in organic synthesis. Such as THF, Et2O, EtOAc, DCM, DMF, DMSO and water etc. etc…. Most of solvent can be easily removed by using rotary evaporator. When I was bench chemist, I like the solvent which has low boiling point. Because it is easy to remove. The solvent which has high boiling point such as DMF, NMP and DMSO is useful and I often use them but don’t like them because difficult to remove after a work-up. Freeze dry is one of useful method for removing these solvents but it takes long time and large equipment.

Following article provides useful approach to remove solvent at ambient-temperature.
A Versatile Method of Ambient-Temperature Solvent Removal

As you can see in the abstract showed above the equipment is very simple. Just only distillation flask and receiver connected narrow glass tube with vacuum stop cock.

After pumping, the receiver chilled with cryogen then solvent will be collected in the receiver.

The author showed some examples, in Fig. 6 showed NMR spectra of benzophenone recovered from DMSO (20mL) and NMP(20mL). Boch chart shows almost pure benzophenone. Both solvents are removed by this method within 50 min at ambient temperature.

Hmm, it seems very useful for small scale synthesis. The equipment is not commercially available but I think it worth to order to make for chemist.

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Published by iwatobipen

I'm medicinal chemist in mid size of pharmaceutical company. I love chemoinfo, cording, organic synthesis, my family.

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