Enhanced resolution in MAS NMR for combinatorial chemistry

Tetrahedron Letters

Volumn 38, Issue 8, 1997, Pages 1333-1336

  Shapiro, Michael J ^a   Chin, Jefferson ^a   Marti, Roger E ^a   Jarosinski, Mark A ^a  

^a Sandoz Pharma Ltd   (Switzerland)

Author keywords

[No Author keywords available]

Indexed keywords

ISOLEUCINE;

ARTICLE; DRUG STRUCTURE; NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY; TECHNIQUE;

EID: 0031584930     PISSN: 00404039     EISSN: None     Source Type: Journal    
DOI: 10.1016/S0040-4039(97)00092-0     Document Type: Article

References (10)

1. 1. a) Fitch, W. L. ; Detre, G.; Holmes, C. P.; Shootery, J. N.; Keifer, P. A. J. Org. Chem. 1994, 59, 7995-7996.
2. b) Shapiro, M. J.; Kumaravil, G.; Petter, R. C.; Beveridge, R. Tetrahedron Letters 1996, 37, 4671-4674.
3. 2. Van, B.; Kumaravet, G.; Anjaria, H.; Wu, A.; Petter, R.; Jewell, C. F., Jr.; Wareing, J. R. J. Org. Chem. 1995, 60, 5736-5738.
4. 3. Anderson, R. C.; Shapiro, M. J.; Stokes, J. P. Tetrahedron Letters 1995, 36, 5311-5314.
5. 4. Anderson, R. C.; Jarema, M. A.; Shapiro, M. J.; Stokes, J. P.; Ziliox, M. J. Org. Chem. 1995, 60, 2560-2651.
6. 5. Keifer, P. J. Org. Chem.. 1996, 61, 1558-1559.
7. 6. Hahn, E. L. Phys. Rev. 1950, 80, 580.
8. 7. Aue, W. P. ; Bartholdi, E.; Ernst, R. R. J. Chem Phys. 1976, 64, 2229.
9. 8. Patek, M.; Lehl, M. Tetrahedron Letters 1991, 32, 3891-3894.
10. 9. All NMR data were collected on a Broker DRX-500 NMR system equipped with a high resolution 4mm MAS probe with a spinning speed of 3500KHz. 3-5 mg of resin containing compound was swelled with an appropriate solvent. All data wasobtained using standard solution pulse programs. The spin echo data was collected using a 70ms echo and the 2D J-resolved data was obtained with a 4K by 32 data matrix optimized for 50 Hz coupling in F1. Typically 32-64 transients were obtained for each increment and the data was processed in the magnitude mode with an unshifted sine window function in both dimensions.