This report outlines a rapid, reproducible method for the determination of beta-asarone, a known carcinogen, using micellar electrokinetic capillary chromatography (MEKC)-UV-vis absorbance and a simple alcohol extraction. The MEKC method is based on a running buffer comprised of 100 mM sodium dodecyl sulfate (SDS), pH 10. The method is reproducible and provides baseline separation of alpha-asarone and beta-asarone. This protocol was used to determine the beta-asarone content of Acorus calamus rhizome of a diploid variety harvested from the wetlands of the United States and the triploid variety from India obtained commercially. The results indicate raw product that originated from India contained 4.4% w/w beta-asarone, while that from the United States contained 0.2% w/w beta-asarone. Neither sample contained detectable concentrations of alpha-asarone. This is the first report of the use of MEKC to determine asarone in a natural source.

A novel route to cyclopenta[b]quinoline-1-ones and-ols has been developed. Substituted cyclopenta[b]quinolin-1-ones were prepared by thermal ringexpansion of substituted N-BOC protected 4-(2-aminophenylethynyl)-4-hydroxy-2-cyclobuten-1-ones forming the corresponding 2-aminophenylmethylidene substituted 4-cyclopentene-1,3-diones. Deprotection of the amine resulted in spontaneous condensation to give cyclopenta[b]quinolin-1-ones. Sodium borohydride reduction of these products produced cyclopenta[b]quinolin-1-ols. The key step in the sequence is a thermally induced ring-expansion of 4-(2aminophenylethynyl)-4-hydroxy-2-cyclobuten-1-ones. Changing the amino protecting group had no effect on the ring size selectivity of the thermal ring expansion. The thermal ring expansion of the corresponding nitro derivative suggests that electron withdrawing substituents may alter the selectivity of the ring formation. The attempted base mediated, copper mediated, copper catalyzed and palladium catalyzed indolization reaction were not further examined since the desired products were not obtained. The N-iodosuccinimide, N-chlorosuccinimide mediated and palladium catalyzed ring expansion reactions Part I A Novel Entry to Cyclopenta[b]quinolines via Thermal Ring-Expansion of (2-Aminophenyl)-Ethynyl-Substituted Cyclobutenone Derivatives

Fused pyridine derivatives R 0450 A Novel Entry to Cyclopenta[b]quinolines via Thermal Ring-Expansion of (2-Aminophenyl)-ethynyl-SubstitutedSquaric Acid Derivatives. -(ZEHR, P. S.; KAYALI, R.; PENA-CABRERA, E.; ROBLES-RESENDIZ, O.; VILLANUEVA-RENDON, A. D.; SOEDERBERG*, B. C. G.; Tetrahedron 64 (2008) 22, 5336-5344; Dep. Chem., W. Va. Univ., Morgantown, WV 26506, USA; Eng.) -Klein 42-131

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