Reaction titration: a convenient method for titering reactive hydride agents (Red-Al, LiAlH4, DIBALH, L-Selectride, NaH, and KH) by No-D NMR spectroscopy.
The concentration of reactive metal hydride (Met-H) reducing agents can be determined (in < or = 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.
Hoye
Thomas R
TR
Department of Chemistry, 207 Pleasant Street, SE, University of Minnesota, Minneapolis, Minnesota 55455, USA. hoye@chem.umn.edu
Aspaas
Andrew W
AW
Eklov
Brian M
BM
Ryba
Troy D
TD
D006859:Hydrogen / Q000737:chemistry*; D007202:Indicators and Reagents / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy / Q000295:instrumentation* / Q000379:methods*; D015394:Molecular Structure; D017186:Titrimetry
D007202:Indicators and Reagents; D006859:Hydrogen