核磁必备文献 JOC NMR Chemical Shifts.pdf

7512 J. Org. Chem. 1997, 62, 7512-7515 NMR Chemical Shifts of Common Laboratory Solvents as Trace Impurities Hugo E. Gottlieb,* Vadim Kotlyar, and Abraham Nudelman* Department of Chemistry, Bar-Ilan University, Ramat-Gan 52900, Israel Received June 27, 1997 In the course of the routine use of NMR as an aid for organic chemistry, a day-to-day problem is the identifica- tion of signals deriving from common contaminants (water, solvents, stabilizers, oils) in less-than-analyti- cally-pure samples. This data may be available in the literature, but the time involved in searching for it may be considerable. Another issue is the concentration dependence of chemical shifts (especially 1H); results obtained two or three decades ago usually refer to much Figure 1. Chemical shift of HDO as a function of tempera- more concentrated samples, and run at lower magnetic ture. fields, than today’s practice. 1 13 We therefore decided to collect H and C chemical dependent (vide infra). Also, any potential hydrogen- shifts of what are, in our experience, the most popular bond acceptor will tend to shift the water signal down- “extra peaks” in a variety of commonly used NMR field; this is particularly true for nonpolar solvents. In solvents, in the hope that this will be of assistance to contrast, in e.g. DMSO the water is already strongly the practicing chemist. hydrogen-bonded to the solvent, and solutes have only a negligible effect on its chemical shift. This is also true Experimental Section for D2O; the chemical shift of the residual HDO is very NMR spectra were taken in a Bruker DPX-300 instrument temperature-dependent (vide infra) but, maybe counter- (300.1 and 75.5 MHz for 1H and 13C, respectively). Unless