I have been reading a bunch of different methods people dry THF, some descriptive, some not. One of which using CaH2 is as follows:
Tetrahydrofuran, b.p. 65.4°
As THF is completely miscible with water it is best not to take any chances as to it being wet. THF should be first refluxed 24 hours over calcium hydride (10 g per liter) then distilled for use in the ketyl pot. Sodium preparation is similar to that for diethyl ether, the final wash of course would be with THF. THF's ketyl is a deep purple color.So im not to sure what this "ketyl pot" is but im guessing it has something to do with the further drying of benzophenone and sodium wire. I then read that some people dry their THF using KOH, and then this benzophenone/sodium mix, however it is unclear to myself how they dry the THF in KOH. Is it refluxed also, then distilled out, or dried over, as with anhydrous magnesium sulfate when drying methanol?
This removal of H2o in THF seems to be a world wide headachs as I read many comments about people having trouble obtaining anhydrous THF, mainly due to the inconsistencies in purity from suppliers. I have some KOH, some benzophenone, yet no sodium wire, can NaCl be used in replace of sodium wire??
Maybe the KOH would be enough if repeated numerous times? My THF isn't
dangerously wet, as a rxn was performed using THF that was dried over MgS04 (2x) and as I have learned, that didn't do anything in removal of moisture.. so I may have well not even bothered and used the THF straight. Yields were horrific so it has to be dried heavily this time to eliminate that factor. Ahh well.. back to the drying board.