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Topic: How can I remove DMSO?  (Read 29368 times)

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Offline peptideismylife

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How can I remove DMSO?
« on: June 07, 2011, 07:22:05 PM »
Hey guys,

How can I remove DMSO? I put it in the roti but it doesnt remove it....

Offline uglepik

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Re: How can I remove DMSO?
« Reply #1 on: June 07, 2011, 07:32:01 PM »
Rotavap will not remove it, even at high bath temperatures.

You need to put on high vacuum (oil pump) and preferably heat it slightly if your compound can tolerate it.

As far as I know azeotropic distillation is not possible.

Offline zaphraud

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Re: How can I remove DMSO?
« Reply #2 on: June 07, 2011, 09:52:21 PM »
Rotavap will not remove it, even at high bath temperatures.

You need to put on high vacuum (oil pump) and preferably heat it slightly if your compound can tolerate it.

As far as I know azeotropic distillation is not possible.

you also might be able to reduce the bulk of it by fractional recrystallization - DMSO has a pretty high MP.. question is if your compound forms a complex crystal with DMSO or separates out as DMSO cools, separates out, or if DMSO separates out and DMSO+compound remains a liquid above that.

Offline poorstudent83

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Re: How can I remove DMSO?
« Reply #3 on: June 08, 2011, 01:10:10 AM »
Is your compound soluble in any chlorinated solvents (DCM or choroform??). Try diluting the DMSO with water then extracting with DCM or chloroform.

Offline Dan

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Re: How can I remove DMSO?
« Reply #4 on: June 08, 2011, 03:45:01 AM »
If your compound is quite low in polarity you can wash it out, as mentioned already.

I usually dissolve in EtOAc and wash with 1:1 brine/water a few times. This works very well for DMF - I haven't tried it for DMSO. Note that if you extract with an organic several times you will probably just back-extract all the DMSO, so I'd do aqueous washes as opposed to organic extractions. I'm basing this on my experience with DMF, so it may not transfer exactly.
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Offline Honclbrif

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Re: How can I remove DMSO?
« Reply #5 on: June 08, 2011, 12:17:42 PM »
I've had good luck using the aqueous extraction method. The more water the better. Sometimes a little DMSO will carry over, but that can be fairly easily removed under high vac.

I've also set up a short path vacuum distillation apparatus to get rid of DMSO from solids.
Individual results may vary

Offline medist

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Re: How can I remove DMSO?
« Reply #6 on: July 06, 2011, 05:54:14 AM »
If your compound is less polar then you can try extraction with diethylether and it would be better to have chilled aq. medium. In my case it worked well.

Offline Zainb

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Re: How can I remove DMSO?
« Reply #7 on: July 06, 2011, 09:12:08 AM »
DMSO is a polar solvent dissolve in water so use the DMSO-H2O phase extracted with diethyl ether.

Offline kukurbituril

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Re: How can I remove DMSO?
« Reply #8 on: July 06, 2011, 04:17:51 PM »
It is not my own experience, but my colleague uses brine instead of just water.

Offline adhikary

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Re: How can I remove DMSO?
« Reply #9 on: July 11, 2011, 08:55:37 AM »
If your product is less polar then try with ethyl ether extraction process, If littlebit polar then better EtOAc. In my case I usually isolate with EtOAc extraction and then crystalization. But, if the product is oily or gummy and highly polar then probably high vacuum distilation is the only way.
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Offline AC Prabakar

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Re: How can I remove DMSO?
« Reply #10 on: July 11, 2011, 09:54:47 AM »
Are you using DMSO as solvent for reaction?

Your desired compound is soluble in organic solvent or water?

If you would like to remove by work-up/extraction try the following article's procedure.

Organic Process Research & Development 2007, 11, 160-164

This article will give u exact qty. of DMSO carried over in organic phase as shared by other members!!
Good Luck!

Offline discodermolide

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Re: How can I remove DMSO?
« Reply #11 on: July 11, 2011, 09:58:18 AM »
Why do you keep on re-hashing the same stupid question?
This is the fourth or fifth or even sixth time you have asked this!
Can the moderators not do something here?
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Offline peptideismylife

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Re: How can I remove DMSO?
« Reply #12 on: July 11, 2011, 10:17:57 AM »
Hey discodermolide,

take a look because I have only ask once. Look at the first message...it was from 7th June, the first time that I've asked. So, there are not fifth or even sixth time....please don't lie. It's not my fault if someone answer one month later and you think that is a new topic...


Offline discodermolide

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Re: How can I remove DMSO?
« Reply #13 on: July 11, 2011, 10:28:21 AM »
Hey discodermolide,

take a look because I have only ask once. Look at the first message...it was from 7th June, the first time that I've asked. So, there are not fifth or even sixth time....please don't lie. It's not my fault if someone answer one month later and you think that is a new topic...



Not correct, this question has been asked and answered several times. Most post coming from you.
Development Chemists do it on Scale, Research Chemists just do it!
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Offline peptideismylife

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Re: How can I remove DMSO?
« Reply #14 on: July 11, 2011, 10:33:35 AM »
So show me how many times I asked this question please...

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