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Organocations in Zeolite Synthesis: Fused Bicyclo [l.m.0] Cations and the Discovery of Zeolite SSZ-48

Lee, Greg S. and Nakagawa, Yumi and Hwang, Son-Jong and Davis, Mark E. and Wagner, Paul and Beck, Larry and Zones, Stacey I. (2002) Organocations in Zeolite Synthesis: Fused Bicyclo [l.m.0] Cations and the Discovery of Zeolite SSZ-48. Journal of the American Chemical Society, 124 (24). pp. 7024-7034. ISSN 0002-7863. doi:10.1021/ja011513o.

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A set of zeolite synthesis experiments is described where lattice substitution is varied in the context of the structure of particular structure-directing organocations (at times referred to as templates). In this particular series, the organocations are constructed as members of a fused bicyclo organonitrogen class of compounds, described as having ring construction [l.m.n], where n = 0. We show that these compounds can best be achieved from starting cyclic ketones that are converted to imines via a Beckman rearrangement reaction. A particular approach to the Beckmann reaction works best in our hands. In some instances isomeric organocations are made and separated. Often their use in zeolite synthesis led to different products. There is a high correlation for the space-filling details of the guest organocations and the type of crystalline host lattice developed in the synthesis. In one instance involving isomers of a decahydroquinoline derivative, a new zeolite, SSZ-48, is discovered and contains only one of the isomers. Characterization of the isomers and their use in the zeolites is followed by 13C MAS NMR analyses. Some details of the new zeolite are given and it is shown that a reasonable symmetry operation predicting a 14-ring zeolite could be generated under similar conditions to SSZ-48 (a 12-ring zeolite).

Item Type:Article
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URLURL TypeDescription ItemSupporting Information
Hwang, Son-Jong0000-0002-3210-466X
Davis, Mark E.0000-0001-8294-1477
Additional Information:© 2002 American Chemical Society. Received 21 June 2001. Published online 23 May 2002. Published in print 1 June 2002. We thank a number of other contributors to this study. Dr. Ignatius Chan is thanked for the electron microscopy shown here, and Dr. Ron C. Medrud and Kenneth Ong are thanked for the Beamline powder XRD data. Rod Tanaka ran many of the XRD patterns described here and LunTeh Yuen provided some of the syntheses. Chevron research management, particularly Dr. Susan Bezman, Dr. Georgie Scheuerman, and Dr. Mike Riddle, is thanked for their continued support of the research collaboration between Chevron Research and Caltech. The NMR facility at Caltech was supported by the National Science Foundation under Grant no. 9724240. Artists Kelly and Scott Harvey are thanked for their 3D modeling and animation of SSZ-48.
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Chevron Research and Technology Co.UNSPECIFIED
Issue or Number:24
Record Number:CaltechAUTHORS:20170407-070957668
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Official Citation:Organocations in Zeolite Synthesis:  Fused Bicyclo [l.m.0] Cations and the Discovery of Zeolite SSZ-48 Greg S. Lee, Yumi Nakagawa, Son-Jong Hwang, Mark E. Davis, Paul Wagner, Larry Beck, and Stacey I. Zones Journal of the American Chemical Society 2002 124 (24), 7024-7034 DOI: 10.1021/ja011513o
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:75818
Deposited By: Ruth Sustaita
Deposited On:07 Apr 2017 15:03
Last Modified:15 Nov 2021 16:55

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