Removing Solvent

Schlenk lines allow solvent and other volatiles to be removed without ever exposing the reaction mixture to atmospheric air or moisture. The low pressures offered by a high vacuum pump means that high boiling solvents such as toluene or chlorobenzene can be easily removed at room temperature, which may be crucial for temperature-sensitive compounds. An external liquid nitrogen trap is essential for removing large volumes of solvent and highly recommended for particularly nasty volatiles, or for solvents with freezing temperatures close to room temperature such as benzene or 1,4-dioxane.

Step 1:  Close the stopcock on the Schlenk flask to seal the contents under inert gas and disconnect it from the Schlenk line tubing. Attach the flask to an external solvent trap, then connect the external trap to the Schlenk line and slowly place under vacuum.

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Attaching the Schlenk flask to the external trap.

Step 2: Slowly lower the external trap into a dewar of liquid nitrogen.

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Lowering the trap into a dewar of liquid nitrogen.

Step 3: Slowly open the stopcock on the Schlenk flask, ensuring that the solution is stirring to prevent bumping. It may be necessary to open the tap fully or use a warm water bath to fully remove all solvent or volatiles.

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Opening the stopcock on the Schlenk flask to begin solvent removal.

Step 4: Once all of the solvent has been removed, close the stopcock on the Schlenk flask as well as the Teflon tap or stopcock connecting the external trap to the Schlenk line. Disconnect the Schlenk flask from the external trap and then cycle it back onto the Schlenk line, slowly opening the stopcock when backfilling with inert gas. Disconnect the external trap from the Schlenk line and remove it from the dewar of liquid nitrogen. Allow the solvent/volatiles to thaw before discarding the contents into an appropriate waste container.

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Schlenk flask after removal of solvent.

This same approach can also be used to partially concentrate solutions in vacuo prior to crystallisation.