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A procedure for synthesis of 2‐methoxyphenothiazine (1) has been developed, starting from resorcinol and aniline by condensation, following methylation and cyclization. p‐Toluenesulfonic acid and polysubstituted aromatics were employed as the catalyst of condensation and the solvent of cyclization, respectively, to improve the yield. The use of parallel experiments, statistical experimental design, and multivariate modeling made the total yield of the procedure as high as 74.2%. J. Heterocyclic Chem., (2012).

The thermal gas‐phase reactions of S+, S2+ and S22+ with methane have been explored by using quadrupole‐ion trap (Q‐IT) mass spectrometry complemented by quantum chemical calculations. In contrast to the reactiveness of the S+/CH4 and S22+/CH4 couples as identified by experiment and computation, respectively, the S2+/CH4 couple is inert at ambient temperature. Interestingly, the hydrogen‐atom transfer (HAT) prevails for S+/CH4 and proton‐coupled electron transfer (PCET) for S2+/CH4, while both PCET and hydride transfer (HT) are accessible for S22+/CH4. Multiple factors matter for these processes. The electronic origins of the different reactivities of the three ions have been interrogated.