calimsiz
Joined: 18 Aug 2006
Posts: 1
Location: Purdue University, West Lafayette IN
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 Posted: Sun Aug 20, 2006 11:52 am Post subject: Titering Reactive Hydride Agents by No-D NMR |
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The following method works fine for determining concentration of hydrides.
Selcuk Calimsiz
Purdue University
Department of Chemistry
Lipton research group
West Lafayette, IN 47907
Ps. autogain process sometimes takes 5-10 minutes.
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ORGANIC LETTERS 2005 Vol. 7, No. 11 2205-2208
Thomas R. Hoye,* Andrew W. Aspaas, Brian M. Eklov, and Troy D. Ryba;
Reaction Titration: A Convenient Method for Titering Reactive Hydride Agents (Red-Al, LiAlH4, DIBALH, L-Selectride, NaH, and KH) by No-D NMR Spectroscopy
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abstract
The concentration of reactive metal hydride (Met-H) reducing agents can be determined (in e20 min) using No-D NMR spectroscopy. The
method involves (i) reacting Met-H with an excess of p-methoxybenzaldehyde, (ii) quenching with excess acetic acid, (iii) recording the No-D
NMR spectrum of this homogeneous mixture, and (iv) deducing the concentration of Met-H from the % conversion (as measured by integration).
By a conceptually related method, the titer of the basic alkali metal hydrides KH and NaH can also be determined. |
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