Reaction titration: A convenient method for titering reactive hydride agents (Red-Al, LiAlH4, DIBALH, L-selectride, NaH, and KH) by No-D NMR spectroscopy

Thomas R. Hoye; Andrew W. Aspaas; Brian M. Eklov; Troy D. Ryba

doi:10.1021/ol0506011

Reaction titration: A convenient method for titering reactive hydride agents (Red-Al, LiAlH₄, DIBALH, L-selectride, NaH, and KH) by No-D NMR spectroscopy

Thomas R. Hoye, Andrew W. Aspaas, Brian M. Eklov, Troy D. Ryba

Chemistry (Twin Cities)

Research output: Contribution to journal › Article › peer-review

20 Scopus citations

Abstract

(Figure Presented) The concentration of reactive metal hydride (Met-H) reducing agents can be determined (in ≤20 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.

Original language	English (US)
Pages (from-to)	2205-2208
Number of pages	4
Journal	Organic Letters
Volume	7
Issue number	11
DOIs	https://doi.org/10.1021/ol0506011
State	Published - May 26 2005

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title = "Reaction titration: A convenient method for titering reactive hydride agents (Red-Al, LiAlH4, DIBALH, L-selectride, NaH, and KH) by No-D NMR spectroscopy",

abstract = "(Figure Presented) The concentration of reactive metal hydride (Met-H) reducing agents can be determined (in ≤20 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.",

author = "Hoye, {Thomas R.} and Aspaas, {Andrew W.} and Eklov, {Brian M.} and Ryba, {Troy D.}",

year = "2005",

month = may,

day = "26",

doi = "10.1021/ol0506011",

language = "English (US)",

volume = "7",

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T1 - Reaction titration

T2 - A convenient method for titering reactive hydride agents (Red-Al, LiAlH4, DIBALH, L-selectride, NaH, and KH) by No-D NMR spectroscopy

AU - Hoye, Thomas R.

AU - Aspaas, Andrew W.

AU - Eklov, Brian M.

AU - Ryba, Troy D.

PY - 2005/5/26

Y1 - 2005/5/26

N2 - (Figure Presented) The concentration of reactive metal hydride (Met-H) reducing agents can be determined (in ≤20 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.

AB - (Figure Presented) The concentration of reactive metal hydride (Met-H) reducing agents can be determined (in ≤20 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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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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