Distillation will be one option if your compound is liquid and stable and if your compound is already precipitated then just simple washing with low boiling solvents and keep that solid in low boiling solvents for exchange to remove completely.

Separation of the mixture depends upon the type of mixture which will decide the scheme. Vaccum distillation is good. Lipolization you can remove water. If other conds. are water insoluble extract in chloroform or ethyl acetate. Dimethylacetamide I guess watter soluble.

Checkout notvoodoo. It is a resource for many of these kinds of organic synthesis and purification questions.

If your product is soluble in straight hydrocarbons, e.g. heptane, hexane etc, you can do extraction as DMA is almost immiscible with these straight HCs solvents..

I was able to dilute my sample 10:1 with water and extract in CHCl3.

I found that small batches worked best.

Any emulsions can be broken with saturated NaCl.

My favourite way at the moment is to find a DMA-miscible solvent in which my compound is insoluble and triturate. For small batches I add the DMA solution to a bunch of 2 mL Eppendorf tubes (< half full), then add the new, poor solvent (e.g. Et2O for a very polar compound, water for non-polar) to the mixture and vortex the tubes until a fine suspension is achieved. Centrifuge these until the compound and supernatant separate, then just pour or pipette the liquid away. Repeat this a few times until all the DMA is gone! I then punch a small hole into the lid of each Eppendorf and stick the whole lot in a desiccator to dry. Once dried, you can easily tip the lumps of product into a vial for weighing, and the remaining residue is usually enough to be dissolved directly in your NMR solvent for characterisation.