A BICYCLIC KETONE AS A SOLID-STATE C-13 NMR INTENSITY REFERENCE

被引:7
作者
HALL, RA [1 ]
JURKIEWICZ, A [1 ]
MACIEL, GE [1 ]
机构
[1] COLORADO STATE UNIV, DEPT CHEM, FT COLLINS, CO 80524 USA
关键词
D O I
10.1021/ac00053a009
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
The synthesis and NMR relaxation properties of 4-(N-methylpyrrolidino)bicyclo[3.2.1]octan-8-one triflate (321) are described. The use of (CO)-C-13-enriched 321 as a C-13 intensity reference is justified and demonstrated. The dominant C-13 peak in 321-(CO)-C-13 is 217 ppm, far from most other C-13 chemical shifts of diamagnetlc organic compounds. Hence, this intensity reference peak avoids peak overlap problems for most organic compounds.
引用
收藏
页码:534 / 538
页数:5
相关论文
共 24 条
[1]  
AXELSON DE, 1985, SOLID STATE NUCLEAR
[2]   METHOD FOR THE CLEAVAGE OF OSMATE ESTERS [J].
BARAN, JS .
JOURNAL OF ORGANIC CHEMISTRY, 1960, 25 (02) :257-257
[3]  
BRYSON RL, 1983, MACROMOLECULES, V16, P1669, DOI 10.1021/ma00244a021
[4]   DYNAMICS OF CROSS RELAXATION IN NUCLEAR MAGNETIC DOUBLE-RESONANCE [J].
DEMCO, DE ;
TEGENFELDT, J ;
WAUGH, JS .
PHYSICAL REVIEW B, 1975, 11 (11) :4133-4151
[5]   FOURIER TRANSFORM STUDY OF NMR SPIN-LATTICE RELAXATION BY PROGRESSIVE-SATURATION [J].
FREEMAN, R ;
HILL, HDW .
JOURNAL OF CHEMICAL PHYSICS, 1971, 54 (08) :3367-&
[6]  
Gerstein B.C., 1985, TRANSIENT TECHNIQUES
[7]  
Hatcher P. G., 1985, Humic substances in soil, sediment and water: geochemistry, isolation and characterization., P275
[8]   HIGH-RESOLUTION NUCLEAR MAGNETIC-RESONANCE OF SOLIDS [J].
MACIEL, GE .
SCIENCE, 1984, 226 (4672) :282-288
[9]   The Claisenic acid cyanide-synthesis. [J].
Mauthner, F .
BERICHTE DER DEUTSCHEN CHEMISCHEN GESELLSCHAFT, 1909, 42 :188-195
[10]  
MEHRING M, 1983, HIGH RESOLUTION NMR, P153