IP Library Granted Patent US 10,040,811
Granted Patent B2
US 10,040,811 · App. 14/387,520 · Granted Aug 7, 2018

Multi-element standard for nuclear magnetic resonance spectroscopy

Inventor: Bernd Willi Karl-Heinz Diehl (Cologne, DE)
Assignee: Merck Patent GmbH
C07F9/36C07F9/094C07F9/12C07F9/3282G01N24/087G01R33/58G01R33/4633
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Quick Facts
Patent No.
US 10,040,811
App. No.
14/387,520
Granted
Aug 7, 2018
Kind
B2
Abstract

Organic compounds which contain nitrogen, fluorine, and phosphorus atoms together with carbon atoms and hydrogen atoms and which can be used as a multi-element standard for 1 H—, 13 C—, 15 N—, 19 F—, and 31 P nuclear magnetic resonance spectroscopy. Also, a nuclear magnetic resonance spectroscopy method, preferably a quantitative nuclear magnetic resonance spectroscopy method, using said compounds and a method for qualitatively and/or quantitatively determining an analyte using such a nuclear magnetic resonance spectroscopy method.

Claims (25)

1. A method of identifying an analyte wherein the method comprises:

providing a standard compound for nuclear magnetic resonance spectroscopy, the standard compound comprised of the formula (1) or (2)

where R 1 is a phenyl radical or benzyl radical whose benzene ring has the following substituents:

at least one —CF 3 substituent,

at least one nitrogen-containing substituent selected from —NO 2 and —NR 4 R 5 , where R 4 and R 5 independently of one another are selected from H, CH 3 , and CH 2 CH 3 , optionally one or two substituents selected from Cl, Br, I, —CH 3 , and —C(═O)OR 6 , where R 6 is selected from H, CH 3 , and CH 2 CH 3 , and

at least one hydrogen atom, where at least one of the hydrogen atoms is ortho to at least one substituent selected from —NO 2 and —C(═O)OR 6 , and

where R 2 and R 3 are the same as R 1 or independently of one another are selected from H, CH 3 , and CH 2 CH 3 ;

detecting the nuclear magnetic resonance of one of the atoms 1 H, 13 C, 15 N, 19 F, or 31 P; and

determining the analyte quantitatively.

2. The method according to 1 , wherein the benzene ring carries precisely two hydrogen atoms as substituents.

3. The method according to claim 2 , wherein the two hydrogen atoms are meta to one another on the benzene ring.

4. The method according to claim 1 , wherein at least one hydrogen atom on the benzene ring is ortho to at least one CF 3 substituent or CH 3 substituent.

5. The method according to claim 1 , wherein at least two hydrogen atoms on the benzene ring are ortho to at least one CF 3 substituent or CH 3 substituent.

6. The method according to claim 1 , wherein at least two hydrogen atoms on the benzene ring are ortho to at least one substituent selected from —NO 2 and —C(═O)OR 6 .

7. The method as claimed in claim 1 , wherein the benzene ring carries only one hydrogen atom as substituent, and the hydrogen atom on the benzene ring is preferably ortho to at least one CF 3 substituent or CH 3 substituent.

8. The method according to claim 1 , wherein, in a 1 H nuclear magnetic resonance spectroscopy, with the chemical shift of tetramethylsilane set as 0 ppm, the chemical shift δ of at least one hydrogen atom on the benzene ring is at least 8 ppm.

9. The method as claimed in claim 8 , wherein the spin-lattice relaxation time T 1 of the at least one hydrogen atom having the chemical shift of at least 8 ppm is not more than 5 s.

10. The method according to claim 8 , wherein the chemical shift of two hydrogen atoms on the benzene ring is at least 8 ppm, and the relaxation times of the two hydrogen atoms differ by at least 3 s.

11. The method according to claim 1 , wherein the compound is selected from the compounds having the formulae (3) to (8):

where the radicals R 2 and R 3 independently of one another are selected from the phenyl radical or benzyl radical shown in the respective formulae, H, CH 3 , and CH 2 —CH 3 , preferably from the phenyl radical or benzyl radical, H, and CH 3 .

12. The method according to claim 11 , wherein the compound is selected from the following compounds:

13. A method of identifying an analyte wherein the method comprises:

providing a standard compound for nuclear magnetic resonance spectroscopy, the standard compound comprised of the formula (9)

detecting the nuclear magnetic resonance of one of the atoms 1 H, 13 C, 15 N, 19 F, or 31 P; and

determining the analyte quantitatively.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 16, 2018
From: DIEHL, BERND WILLI KARL-HEINZ
To: MERCK PATENT GMBH
Reel/Frame 044953/0987 →
Priority Claims (1)
DE 10 2012 204 701 · Mar 23, 2012 · national
Continuity (1)
Related Publication 20150077104A1 · Mar 19, 2015
Cited By (1)
US 12,571,867