Distillation under reduced pressure

Depending on the kinetic solubility of the resin you can simply wash it with 1:1 ethanol/water solvent mixtures, the DMF should be displaces and the loss of resin should be low. If the solubility of the resin is high, besides you can make methanol/hexane or CHCl3/H2O partitions and look forward to displace your resin into the hexanes or CHCl3 and leave DMF in methanol or water. Otherwise use liquid-liquid extraction apparatus with CHCl3/H2O or methanol/hexane systems. Use TLC to track enrichment of one specific fraction.

Try with lyophliser... Coling with liq. Nitrogen and vaccum evopration... or else by distillation in reduced pressure.

I am agree with Subramanian's view lypholiser is a good choice. if you have this facility available then go for it.

But removing DMF under reduced pressure require a high capicity vaccum pump and some time also high degree of temperature also require, so if a compound is not thermally stable then you may lose it.

you can also try in a small scalle -take a reaction mixture ( known amount) dilute it with minimum 10-12 times with ice cold water and try to extract the product by using different water immissible solvent. I have used this method several time for the synthesis of hetrocyclic compound.

hope it will work in your case as well.

good luck.

If you do not have a lyophiliser, you can put your product under vaccum (a standard mecanical pump is enough) with a gentle heating (ca. 40-60°C) for a few hours. That should be enough to remove almost all the DMF.

I would try washing with water first, several times (6 times), the DMF should go into the water. If the resin is solid try to grind it up as small as you can. if its a gel maybe sonication. After you have taken the water away by filtration or decantation, add benzene and evaporate the azeotrope out under reduced temperature and mild heating (two or three times). This should do the trick. Good luck!

I would try to well wash the resin with brine followed by water and dry. Depending of the solubility of the resin you could also, after the water wash with ethanol. Good luck

In order to remove DMF from polymers I dissolve the polymer in a suitable solvent and add water. Then I remove the mixture of solvent, DMF and water on rotary evaporator.

Look for DMF-water or DMF-tolune azeotrope. Add toluene at the end of the distillation. That should solve the problem.

Try adding water to the mixture and extract with low polarity solvent like ether. There would be some DMF extracted along with your product and to remove it wash the combined etheral extracts with a saturated aqueous solution of NaCl.

you can remove DMF from the product by adding water then, evaporate under vacuum carefully

If your copound is soluble in organic solvent (not in alcohols, acetones), add saturated NaCl solution to the compound and extract the compound from it. You can get rid off DMF by repeating this process 3-4 times.

Good luck!

The best (and simplest) way is to dissolve your compound in ethyl acetate and wash with H2O. It works fine with medium polarity compounds. If you suspect that your compound may be partially soluble in H2O then wash with aqueous NaCl

The crude reaction mixture is poured into saturated aqueous NH4Cl solution (R.M. X 4, by volume), followed by extraction (X 2) with suitable solvent (Et2O, EtOAc…). The combined organic layer is washed one more time with satd. aq. NH4Cl.

BW

dmf removal require high vacuumed distillation followed by extraction of product in organic phase

You can use heptane or even water for the co-evaporation of DMF..

In my experience co-evaporation of DMF with water works well even at 45-50 oC.

All the above ans are good aswell i think you con't distill it so quench it 13-15 times of water at your reasonable temp (15-25)  and extract that with immiscible solvent distill out the solvent at your appreciative temp  

Wash the product mixture with water. Further, to create distinct layers in the separating funnel, you can add NaCl. Repeat the process several times for better result. Thenevaporate and load!

what about dmf trapped in crystal pl suggest

Hello Erigene,

this is my advise to remove DMF from water-soluble compounds which are NOT or insufficiently extractable into organic phases.

I simply heat the solution to 60-70 deg. Celsius and apply a gentle air flow (or nitrogen or argon). Typically, I place my solution (water-DMF or DMF only) in a 10mL glass vial and insert a 1mL syringe attached to an air/N2/Ar source. Keep an appropriate distance of syringe to surface of solution to avoid spilling. With this procedure I evaporate DMF in no time compared to "rotavaping". The remove traces I redissolve the almost dry residue in water and lyophilize it.  

Be carefully with temperature-sensitive compounds.

DMF is water soluble. so, simply add water and organic phase (ethyl acetate or DCM-based on solubility of your compound). Don't shake vigorously, due to vigorous shaking total content shows turbidity. DMF soluble in water and you desired compounds comes in to ethyl acetate. Evaporate ethyl acetate to get your desired compound.

DMF doesn't form an azeotrope with heptane. They are not even miscible.

I think DMF/xylene form aziotrope; please check though. 

If the DMF was used as the solvent for the reaction, it is usually preferable to almost  dry it completely off in a high vac before washing with water and NaCl which will take up the residual DMF in the product. Else, one would lose a sizeable quantity of one's product, since the product, in most cases, will be appreciably soluble in the organic solvent used for the extraction as well as in the residual DMF which will form a turbid layer in-between the organic and aqueous phases.

bonjour,

pour éliminer le DMF il faut travailler avec un système T, car cette technique est utilisé pour éliminer les solvants non volatile, ci-joint tu trouveras le schéma

For 5 mL of DMF or DMSO, I use 5 X 10 mL of water during the aqueous wash. This should remove all of the DMF or DMSO.

Then two aqueous washes to remove DMF:

1. 5% LiCl (aq)

2. 0.5 N HCl

better to distill off dmf with azeotropic distillation using toluene &treat   residue with water

otherwise compound will be lost in dmf -water

Upon heating the dmf,  whether dmf gets solidified or evaporates  ? 

In Case of polymer wash with Methanol followed by ether it pretty well. and dry under vacuum, it is good especially in PS-DVB based polymer. gooood luck  

Can heat up to 120 C in the oven, if you keep on, resin can degrade because it can consist styrene in resin mixture. Dont forget DMF's boils at 150 C. Thats why u have to arrange the time that you will apply.

Add some ice cold water (ratio 1:5 = DMF/Ice cold water) to the reaction mixture and shake it thoroughly for few minutes (2 min.). After that, add some saturated brine solution and organic solvent to the mixture shake it well for few minutes. Then, I hope you will get good layers in the separating funnel. This procedure has to repeat 3 to 4 times.

If your product is soluble in ether or EtOAc then wash the organic layer with water (once or twice) then with brine (3-4 times). DMF will wash away. Another method is to wash your organic layer with 5% LiCl several times. These work fine.

I did many reactions in DMF and this is how I always perfectly got rid of it from my products without distilling: repeated extractions diethyl ether/water. DMF does not mix with Et2O very well so if your product is soluble in this solvent, you can dissolve it and then extract 4-5 times with water. Be careful not to use too much Et2O, otherwise you end up with some DMF in it. Good luck!

Reapeted distillation with toluene is IMHO the best choice, not only removes DMF but also water. U can do this by simply adding 3-5 volumes of toluene to your flask with DMF solution, concentrating mixture by rotary evaporation and repeating this two steps until there is no DMF/water left. Works great, but only for non-volatile products.

Otherwise you can try extraction. Washing organic (for instance AcOEt) layer with LiCl solution (10% in water) should remove most DMF quite nice. Works great, but only for water insoluble products.

Distillation under strong vacuum pump

Otherwise, if your product is not soluble in water, washing with a mixture EtOH-water (1÷1) should work

Liquid-liquid extraction (EtOAc-citric acid) works well in the case your compound is soluble in EtOAc

Last but not the least column chromatography, Dmf will be trapped by silica

Good luck!