This contribution describes a general method
for the purification of solvents for use with air and
moisture sensitive reactions. This procedure provides
a
nonhazardous alternative to distillations and vacuum
transfers and does not require undue supervision or
cooling, yet allows for the rapid collection of large
quantities of extremely pure solvents on demand. Solvents are rigorously degassed in 18 L reservoirs and
passed through two sequential purification columns.
Protic contaminants are removed with activated alumina, while a supported copper catalyst is used to
remove trace oxygen from hydrocarbons. The purification system is interfaced with either a glove box or
Schlenk manifold for the anhydrous/anaerobic collection
of solvents. Solvents purified by this method and
tested
with stock solutions of sodium benzophenone ketyl or
titanocene dichloride/zinc dust are free of oxygen at
least
to the ppm level. Furthermore, this system may be
used
for the in-line purification of gases and is easily scaled
down to provide a convenient method for the purification
of deuterated solvents or other reagents.
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