Herein, we report the first synthesis of chlorinated benzo[b]selenophenes via environmentally friendly electrophilic chlorocyclization reaction using “table salt” as a source of “electrophilic chlorine” and ethanol as a solvent. In addition, the synthesis of diverse halogenated heterocycles, including 3-chloro, 3-bromo and 3-iodo thiophenes, selenophenes, and benzo[b]selenophenes was successfully accomplished under the same environmentally benign reaction conditions. This methodology has several advantages over other previously reported reactions as it employs simple starting compounds, an environmentally friendly solvent, ethanol, and non-toxic inorganic reagents under mild reaction conditions, resulting in the high product yields.

Details of coupling a catalytic reaction chamber to a liquid nitrogen-cooled cryofocuser/triple quadrupole mass spectrometer for online monitoring of nitric oxide (NO) photocatalytic reaction products are presented. Cryogenic trapping of catalytic reaction products, via cryofocusing prior to mass spectrometry analysis, allows unambiguous characterization of nitrous oxide (N 2 O) and nitrogen oxide species (i.e., NO and nitrogen dioxide (NO 2)) at low concentrations. Results are presented, indicating that the major photocatalytic reaction product of NO in the presence of titanium dioxide (TiO 2) P25 and pure anatase catalysts when exposed to ultraviolet (UV) light (at a wavelength of 365 nm) is N 2 O. However, in the presence of rutile-rich TiO 2 catalyst and UV light, the conversion of NO to N 2 O was less than 5% of that observed with the P25 or pure anatase TiO 2 catalysts.

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We demonstrated that the use of high-frequency QIGs can extend the operational lower m/z range for both external EI- and ESI-FTICR mass spectrometers. By considering both ICR and Mathieu equations of motions to describe ion trajectories, theoretical ion ejection thresholds (consistent with our experimental findings) could be predicted.