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THF的处理.pdf
Ver. 8/2009 CMP/WO
The Benzophenone/Ketyl Tetrahydrofuran(THF) Still
1. Introduction
The benzophenone-sodium still is a widely used method to produce moisture, oxygen, and peroxide free
organic solvents, especially for tetrahydrofuran (THF). The soluble benzophenone ketyls can be formed
as radical anion by one-electron reduction of carbonyls with sodium. The ketyl molecule is intensively
colored (deep blue) and reacts quickly with the water, oxygen, and peroxide dissolved in organic
solvents. The deep blue coloration indicates dry and oxygen free conditions. (Schwartz, A. M. Chem. Eng.
News 1978, 24, 88.)
2. Before getting started
Appropriate safety measures should be inplaces during all steps of solvent distillation. The largest
danger with this distillation is fire due to spillage. THF is quite flamable and THF vapor is about two and
a half times the density of air. Be aware of the risks inherent to the reaction you will perform and
appropriate countermeasures. Do you know where the nearest chemical shower is located? Sodium
metal is reactive to water and it is recommended to have a 500 mL beaker of isopropyl alcohol to
remove small pieces of sodium generated during chopping. At least one carbon dioxide or dry-chemical
fire extinguisher should be readily available when working with sodium. Perform all wo rk inside an
operating fume hood.
The distillation setup pictured to the left is fairly common.
The boiling flask 1 is a 3000 mL, two necked variety with
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