I was synthesizing a couple of compounds at a reaction temperature of 80 °C. Both are very likely to be water-soluble, and so extracting the DMF into the water phase was not an option. Elsewhere I read a suggestion to use 3:2 toluene and rotary evaporation. I had to do this about four times for each crude reaction and use a high temperature bath, but eventually I got rid of the majority of the mass, presumably the DMF. Possibly with a higher ratio of toluene, I would have needed fewer evaporations.