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Synthesis and X-ray diffraction data of 7-methyl-cis-2-(1’-naphthyl)-2,3,4,5-tetrahydro-1H-benzo[b]azepin-4-ol

Published online by Cambridge University Press:  06 March 2012

M. A. Macías
Affiliation:
Grupo de Investigación en Química Estructural (GIQUE), Escuela de Química, Facultad de Ciencias, Universidad Industrial de Santander, A.A. 678, Carrera 27, Calle 9 Ciudadela Universitaria. Bucaramanga, Colombia
J. A. Henao*
Affiliation:
Grupo de Investigación en Química Estructural (GIQUE), Escuela de Química, Facultad de Ciencias, Universidad Industrial de Santander, A.A. 678, Carrera 27, Calle 9 Ciudadela Universitaria. Bucaramanga, Colombia
Carlos Mario Sanabria
Affiliation:
Laboratorio de Síntesis Orgánica (LSO), Facultad de Ciencias, Universidad Industrial de Santander, A.A. 678, Carrera 27, Calle 9 Ciudadela Universitaria. Bucaramanga, Colombia
Alirio Palma
Affiliation:
Laboratorio de Síntesis Orgánica (LSO), Facultad de Ciencias, Universidad Industrial de Santander, A.A. 678, Carrera 27, Calle 9 Ciudadela Universitaria. Bucaramanga, Colombia
*
a)Author to whom correspondence should be addressed. Electronic mail: [email protected]

Abstract

The 7-methyl-cis-2-(1’-naphthyl)-2,3,4,5-tetrahydro-1H-benzo[b]azepin-4-ol (chemical formula C21H21NO) was prepared via the reductive cleavage of the bridged N-O bond of the corresponding 7-methyl-2-exo-(1′-naphthyl)-1,4-epoxytetrahydro-1-benzazepine. The X-ray powder diffraction pattern for the new compound was analyzed and found that the title compound crystallizes in a monoclinic system with space group P2/c (No. 13) and refined unit-cell parameters a = 11.012(2), b = 18.613(5), c = 7.316(4) Å, β = 102.88(3) ° and V = 1461.8(7) Å3.

Type
New Diffraction Data
Copyright
Copyright © Cambridge University Press 2011

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References

Buhrke, V., Jenkins, R., and Smith, D. (1998). Preparation of Specimens for X-Ray fluorescence and X-ray Diffraction Analysis (Wiley, New York), pp. 141142.Google Scholar
Boultif, A. and Loüer, D. (2006). “Indexing of powder diffraction patterns of low symmetry lattices by successive dichotomy method,” J. Appl. Crystallogr. 37, 724731.10.1107/S0021889804014876CrossRefGoogle Scholar
de Wolff, P. M. (1968). “A simplified criterion for the reliability of a powder pattern,” J. Appl. Crystallogr. 1, 108113.10.1107/S002188986800508XCrossRefGoogle Scholar
Dong, C. (1999). “POWDERX: Windows-95-based program for poder X-ray diffraction data processing,” J. Appl. Crystallogr. 32, 838838.10.1107/S0021889899003039CrossRefGoogle Scholar
Gómez-Ayala, S., Castrillón, J. A., Palma, A., Leal, S. M., Escobar, P., and Bahsas, A. (2010). “Synthesis, structural elucidation and in vitro antiparasitic activity against Trypanosoma cruzi and Leishmania chagasi parasites of novel tetrahydro-1-benzazepine derivatives,” Bioorg. Med. Chem. 18, 47214739.10.1016/j.bmc.2010.05.018CrossRefGoogle ScholarPubMed
Gómez-Ayala, S. L., Stashenko, E., Palma, A., Bahsas, A., and Amaro-Luis, J. M. (2006). “Sequential amino-claisen rearrangement/intramolecular 1,3-dipolar cycloaddition/reductive cleavage approach to the stereoselective synthesis of cis-4-hydroxy-2-aryl-2,3,4,5-tetrahydro-1(1H)-benzazepines,” Synlett 14, 22752277.10.1055/s-2006-949654Google Scholar
Laugier, J. and Bochu, B. (2002). “LMGP-suite suite of programs for the interpretation of X-ray. experiments,” CHEKCELL, ENSP/Laboratoire des Matériaux et du Génie Physique, BP 46. 38042 Saint Martin d’Hères, France. http://www.inpg.fr/LMGP and http://www.ccp14.ac.uk/tutorial/lmgp/.Google Scholar
Mighell, A. D., Hubberd, C R., and Stalick, J. K. (1981). “NBS* AIDS80: A FORTRAN program for crystallographic data evaluation,” Natl. Bur. Stand. (U.S.), Tech. Note 1141.CrossRefGoogle Scholar
Palma, A., Yépes, A. F., Leal, S. M., Coronado, C. A., and Escobar, P. (2009). “Synthesis and in vitro activity of new tetrahydronaphtho[1,2-b]azepine derivatives against Trypanosoma cruzi and Leishmania chagasi parasites,” Bioorg. Med. Chem. Lett. 19, 23602363.10.1016/j.bmcl.2008.05.013CrossRefGoogle ScholarPubMed
Rachinger, W. A. (1948). “A correction for the α1 α2 doublet in the measurement of widths of X-ray diffraction lines,” J. Sci. Instrum. 25, 254255.10.1088/0950-7671/25/7/125CrossRefGoogle Scholar
Savitztky, A. and Golay, M. J. (1964). “Smoothing and differentiation of data by simplified least squares procedures,” Anal. Chem. 36, 16271639.10.1021/ac60214a047CrossRefGoogle Scholar
Smith, G. S. and Snyder, R. L. (1979). “F N: A criterion for rating powder diffraction patterns and evaluating the reliability of powder-pattern indexing,” J. Appl. Crystallogr. 12, 6065.10.1107/S002188987901178XCrossRefGoogle Scholar
Sonneveld, E. J. and Visser, J. W. (1975). “Automatic collection of powder diffraction data from photographs,” J. Appl. Crystallogr. 8, 1–7.10.1107/S0021889875009417CrossRefGoogle Scholar