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Author Topic: How to Evaporate DMSO?  (Read 12922 times)

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nkenton

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How to Evaporate DMSO?
« on: October 18, 2011, 05:16:47 AM »

I have an amino acid derivative dissolved in DMSO/water.  I am trying to build a lyophilizer apparatus to attach to my Schlenk line, but I don't know the best equipment to use.  Furthermore, I do not know the names of the glassware pieces I need to procure.  Price is also a factor.

Can someone help me?
« Last Edit: October 18, 2011, 05:57:42 AM by Mitch »
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Mitch

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Re: evaporating DMSO
« Reply #1 on: October 18, 2011, 05:53:41 AM »

I don't think you can evaporate the DMSO away.
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nkenton

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Re: How to Evaporate DMSO?
« Reply #2 on: October 18, 2011, 08:51:33 AM »

The paper from which I have developed the procedure says the DMSO was evaporated in vacuo.  So someone sometime did it somewhere...  ???

I have a setup I found in Vogel's Practical Organic Chemistry, 5th ed., on page 155, which has two condensers in a line preceding an oil pump.
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Honclbrif

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Re: How to Evaporate DMSO?
« Reply #3 on: October 18, 2011, 11:07:21 AM »

I've shifted small volumes of DMSO with a high vac pump and some heat, but it takes either a really good pump, or a lot of heat (http://www.sigmaaldrich.com/chemistry/solvents/learning-center/nomograph.html).

If your compound is soluble in an organic solvent which is immiscible with water, the best way to get rid of DMSO is to dilute the hell out of the sample with water and do repeated extractions with solvent. Check with TLC to make sure you've got it all. If you're lucky the DMSO will stay in the water, but usually you get a small amt coming along for the ride. You can try vac-ing that smaller amt off.

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fledarmus

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Re: How to Evaporate DMSO?
« Reply #4 on: October 18, 2011, 01:19:56 PM »

We had some high-vac centrifugal evaporators that could remove DMSO (like http://www.genevac.com/en/Index.asp) but on the whole, trying to evaporate off DMSO is a real pain in the... I mean, a real challenge. I find it best to avoid DMSO altogether if you can't extract your final compound away from water.

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SA

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Re: How to Evaporate DMSO?
« Reply #5 on: May 22, 2018, 07:05:49 PM »

My colleagues use Smart Evaporator. It works well to evaporate DMSO and DMF.
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PKa

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Re: How to Evaporate DMSO?
« Reply #6 on: July 21, 2018, 06:49:17 AM »

You should be able to remove few mL of DMSO using a rotovap with a good vaccum pump attached. I have been able to remove around 50 mL of DMSO at around 45-50 oC water bath temperature.
I have also removed DMSO using a Labconco freeze dryer in about overnight time. hope it helps
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