Remarkably, F NMR analysis of the irradiated sample revealed partial conversion of the diazirine to a mixture of the desired C-H insertion product 7 (Fig. ) and the corresponding linear diazo isomer (a well-known photo-isomerization product for diazirines). A control sample (maintained in the dark for an equivalent period of time) showed neither the linear diazo isomer nor the C-H insertion product. While the percent conversion in the experiment remained low-a consequence of the fact that the laser irradiated only a small portion of the capillary's total volume-we were able to confirm the presence of adduct 7 from the chemical shift of the new signal (-63.26 ppm in the F NMR spectrum) and from the fact that this signal split into a doublet when 1 H-coupling was enabled during the NMR acquisition (inset to Fig. ). The presence of compound 7 was further confirmed by mass spectrometry.