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Topic: Removing DMF from a sample of a salt.  (Read 3533 times)

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Offline zuriel

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Removing DMF from a sample of a salt.
« on: January 27, 2017, 08:40:04 AM »
Hi everyone,

I have a little problem - I have a very small amount of a salt which I made employing DMF as the solvent. I know water/acid can get rid of DMF but unfortunately I can't use either. I've tried drying my compound under high-vac but to no or little avail. Does anyone know of any other useful tricks to remove DMF from a sample without the use of water or acid?

Cheers

Offline TheUnassuming

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Re: Removing DMF from a sample of a salt.
« Reply #1 on: January 27, 2017, 09:27:13 AM »
Try triturating your sample in organic solvents that are miscible with DMF but in which your salt has little to no solubility.
When in doubt, avoid the Stille coupling.

Offline pgk

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Re: Removing DMF from a sample of a salt.
« Reply #2 on: January 27, 2017, 11:14:48 AM »
Add toluene and distill in the rotary at ≈ 30oC and ≈14/mmHg.
It also works with xylene, heptane and hexane but at slight different temperatures.

Offline zuriel

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Re: Removing DMF from a sample of a salt.
« Reply #3 on: January 29, 2017, 05:01:14 PM »
thanks for the suggestions, I'm going to try a trituration first and see how that goes.  8)

Offline Optimist

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Re: Removing DMF from a sample of a salt.
« Reply #4 on: January 30, 2017, 04:40:55 AM »
If your compound is sensitive to heat the best way to get rid of DMF is using lyophilization process if you have access to freeze dryer.

Add water to your sample and run freeze dryer overnight

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