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Safe and Convenient Procedure for Solvent Purification

Pangborn, Amy B. and Giardello, Michael A. and Grubbs, Robert H. and Rosen, Robert K. and Timmers, Francis J. (1996) Safe and Convenient Procedure for Solvent Purification. Organometallics, 15 (5). pp. 1518-1520. ISSN 0276-7333. doi:10.1021/om9503712.

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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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Grubbs, Robert H.0000-0002-0057-7817
Additional Information:© 1996 American Chemical Society. Received May 22, 1995.
Issue or Number:5
Record Number:CaltechAUTHORS:20180518-145240047
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Official Citation:Safe and Convenient Procedure for Solvent Purification Amy B. Pangborn, Michael A. Giardello, Robert H. Grubbs, Robert K. Rosen, and Francis J. Timmers Organometallics 1996 15 (5), 1518-1520 DOI: 10.1021/om9503712
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:86466
Deposited By: George Porter
Deposited On:21 May 2018 15:41
Last Modified:15 Nov 2021 20:38

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