Giri Nand Gopal, Chauhan Shive Murat Singh
Department of Chemistry, Bio-organic Research Laboratory, University of Delhi, Delhi 110 007, India.
Spectrochim Acta A Mol Biomol Spectrosc. 2009 Sep 15;74(1):297-304. doi: 10.1016/j.saa.2009.06.019. Epub 2009 Jun 16.
The binding studies of calix[4]pyrroles (1-6) with fluoro, chloro, bromo, iodo and sulphato anions generated from normal-tetrabutylammoniumfluoride, normal-tetrabutylammoniumchloride, normal-tetrabutylammoniumbromide, normal-tetrabutylammoniumiodide, and normal-tetrabutylammoniumsulphate respectively were investigated by electrospray ionization mass spectrometry (ESI-MS) in dichloromethane-acetonitrile in negative ion mode. The efficacy of a particular calix[4]pyrrole to bind with anions was found maximum at low cone voltage of the instrument, at high cone voltage the binding was suppressed due to removal of anion from the cavity of the macrocycles. The binding strength was found inversely proportional to the size of anion for a particular calix[4]pyrrole. The fragmentation pattern of calix[4]pyrrole was observed at higher cone voltage of ESI-MS and was interpreted. The association constants of calix[4]pyrroles and anions obtained from electronic transition studies were in good agreement with that observed from (1)H NMR titration studies.
通过电喷雾电离质谱(ESI-MS)在二氯甲烷 - 乙腈的负离子模式下,研究了杯[4]吡咯(1 - 6)分别与由正四丁基氟化铵、正四丁基氯化铵、正四丁基溴化铵、正四丁基碘化铵和正四丁基硫酸铵产生的氟、氯、溴、碘和硫酸根阴离子的结合研究。发现特定杯[4]吡咯与阴离子的结合在仪器的低锥电压下最大,在高锥电压下,由于阴离子从大环腔中去除,结合受到抑制。对于特定的杯[4]吡咯,发现结合强度与阴离子大小成反比。在ESI-MS的较高锥电压下观察并解释了杯[4]吡咯的碎裂模式。从电子跃迁研究获得的杯[4]吡咯与阴离子的缔合常数与从¹H NMR滴定研究观察到的结果高度一致。