For the sulfene study: Experiments were conducted to obtain sulfene at -196°C, observe its infrared spectrum, and follow its reactions—this marks the first direct observation of any sulfene. Modifying the apparatus to use "homogeneous" trapping increased the yield of methyl methanesulfonate from 2.6% to 40% while reducing methanesulfonyl chloride. Using DCl as a trap showed methanesulfonyl chloride derived from sulfene. The infrared spectrum of the thermolysate at -196°C exhibited bands ascribed to sulfene (3170, 3040, 1330, 1230, and 950 cm⁻¹); these bands disappeared on warming and were replaced by the spectrum of methanesulfonyl chloride. Depositing methanol with the thermolysate via the "homogeneous" technique showed sulfene bands that vanished upon warming, replaced by methyl methanesulfonate. Final confirmation came from thermolyzing methanesulfonic anhydride, whose thermolysate at -196°C showed the same characteristic sulfene bands. For the Negamycin study: Negamycin is a new antibiotic isolated from the culture filtrate of Streptomyces purpeofuscus-related strains, possessing strong inhibitory activity against resistant Gram-negative bacteria including Pseudomonas. This work reports its structural elucidation, partial synthesis, and a novel acid-catalyzed rearrangement of 1-methylhydrazinoacetic acid discovered during the study. Acid hydrolysis of negamycin yielded 6-hydroxy-β-lysine, sarcosine, methylamine, 1,2-dimethylhydrazine, and 1-methylhydrazinoacetic acid (which rearranged to 1,2-dimethylhydrazine). The hydrazide structure was confirmed by high-resolution mass spectrometry, and the absolute configuration of the amino acid moiety (L-configuration at the 6-position) was determined using Hudson's lactone rule and Klyne's lactone sector rule, verified by synthesis from a carbohydrate precursor of known configuration. Partial synthesis of negamycin from 6-hydroxy-β-lysine and 1-methylhydrazinoacetic acid produced a compound identical to natural negamycin in all respects, including biological activity.