I want to know the detailed procedure for drying it. I am more interested to use KOH for drying. I want the procedure from starting.
- THF (Tetrahydrofuran): distilled from sodium benzophenone ketyl. Add sodium wire and benzophenone to a volume of THF (pre-dried over calcium hydride or 4A molecular sieves), heat at reflux/under nitrogen for several hours until the solvent turns deep blue in colour. This indicates the solvent is dry, and you can distill off the volume you require. With time (weeks-maybe months if used correctly) the still will turn orange, this indicates that it is time to make a new one!
- https://s3.wp.wsu.edu/uploads/sites/33/2013/10/THF-Still.pdf @
Tetrahydrofuran (THF) should be pre-dried overnight over potassium hydroxide (KOH) or molecular sieves (3 or 4 Å). Extract a block of sodium metal from the container and rinse with a minimum amount of hexanes to remove the oil or kerosene. https://s3.wp.wsu.edu/uploads/sites/33/2013/10/THF-Still.pdf
Add sodium wire and benzophenone to a volume of THF (pre-dried over calcium hydride or 4A molecular sieves), heat at reflux/under nitrogen for several hours until the solvent turns deep blue in colour. This indicates the solvent is dry, and you can distill off the volume you require. https://chem.libretexts.org/Ancillary_Materials/Demos_Techniques_and_Experiments/General_Lab_Techniques/Drying_Solvents
About drying tetrahydrofuran (THF) ― Please check: https://www.researchgate.net/post/Anhydrous-Solvent-How-we-can-dry-solvent https://www.researchgate.net/post/What_are_other_methods_of_drying_THF_without_the_use_of_sodium_wire_and_benzophenone
https://www.researchgate.net/post/Has-anyone-experienced-problems-with-drying-THF-and-diethyl-ether-using-a-solvent-purification-system-MBraun
Dear Aashna Perwin thank you for your interesting technical question. In this context please also have a look at the following potentially useful and unstructive article:
Revisiting of Benzophenone Ketyl Still: Use of a Sodium Dispersion for the Preparation of Anhydrous Solvents
Article Revisiting of Benzophenone Ketyl Still: Use of a Sodium Disp...
(see attached pdf file)
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