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Los clorofullerenos solubles son los siguientes: C ((60) Cl ((2,4,6,8,10). Síntesis, purificación, análisis de
Igor V Kuvychko1, Alexey V Streletskii, Natalia B Shustova
1Department of Chemistry, Colorado State University, Fort Collins, Colorado 80523, USA.
Journal of the American Chemical Society
|April 23, 2010
Resumen
Este estudio revela que muchos métodos analíticos proporcionan resultados inexactos para los fullerenos clorados (C ((60) Cl ((n)). La caracterización óptima implica la cromatografía líquida de alto rendimiento (HPLC) combinada con la espectrometría de masas (MS), lo que permite la síntesis de nuevos compuestos C60) Cln.
Área de la Ciencia:
- Química de los fullerenos.
- Ciencia de los materiales Ciencia de los materiales.
- Química Analítica La Química Analítica es la
Sus antecedentes:
- La caracterización de los fullerenos clorados (C60) es crucial para comprender sus propiedades y aplicaciones.
- Los estudios previos a menudo se basaron en técnicas analíticas que arrojaron resultados ambiguos o erróneos para los compuestos C ((60) Cl ((n).
- La pureza y la composición de muchos derivados de C60) Cl (n) reportados han sido cuestionables debido a limitaciones analíticas.
Objetivo del estudio:
- Evaluar la eficacia de diversas técnicas analíticas para la caracterización de los productos C60) Cln).
- Establecer una metodología analítica óptima para un análisis fiable de C60) Cln.
- Explorar nuevas reacciones de cloración de C ((60)) y caracterizar nuevos compuestos C ((60) Cl ((n)).
Principales métodos:
- Evaluación de RMN, UV-vis, IR, espectroscopia de Raman, varias técnicas de espectrometría de masas (FAB, MALDI, LDI, ESI, APCI), HPLC, TGA, análisis elemental y difracción de rayos X. Se incluyen:
- Estudio detallado de la cloración de C60) utilizando ICl, ICl3 y Cl2 con HPLC dinámico y espectrometría de masas APCI.
- Síntesis y caracterización de nuevos clorofulerenos, incluido el C60) Cl10), utilizando (13) C RMN y difracción de rayos X; se utilizaron cálculos DFT para el análisis estructural.
Principales resultados:
- La mayoría de las técnicas analíticas convencionales proporcionaron datos poco confiables para los compuestos C60) Cln).
- Una combinación de HPLC y espectrometría de masas MALDI o APCI fue identificada como el método analítico óptimo.
- Se han sintetizado y caracterizado con éxito los nuevos clorofullerenos (1,7-C(60) Cl(2), 1,9-C(60) Cl(2), 1,6,9,18-C(60) Cl(4), y 1,2,7,10,14,24,25,28,29,31-C(60) Cl(10).
- Se determinó inequívocamente la estructura asimétrica de C(60) Cl(10) y se racionalizó su mecanismo de formación.
- Se encontró que los clorofullerenos son altamente sensibles a la luz en solución.
Conclusiones:
- La fiabilidad de los métodos analíticos es fundamental para una caracterización precisa de C60) Cln).
- HPLC junto con MS (MALDI o APCI) proporciona un enfoque robusto para el análisis de los clorofullerenos.
- Esta investigación amplía la familia conocida de compuestos C60) Cln) y destaca su sensibilidad a la luz.
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