Fig. 8: Stoichiometric palladium reactivity studies using substrate 1a.
From: Deciphering complexity in Pd–catalyzed cross-couplings
31P NMR (203 MHz, DMF-d7) spectral changes and confirmation of derived (pseudo)molecular ions by ESI-MS: (1) Pd2dba3·CHCl3 and dppe taken at rt, t = 0 min; (2) taken after addition of 2-bromo-benzamide 1a at rt, t = 5 min; (3) taken after 45 min heating at 80 °C; (4) taken after 16 h heating at 80 °C. We have assigned species to five phosphorus species, cross-referenced with the ESI-MS analysis (simulated ions shown in red; experimental ions in blue). The species at δ 57.35 is a trace product, derived from the formation of Pd0(dba)(dppe)/Pd0(dppe)2, which is distinct to the species at δ 56.77 ppm, formed at higher temperature, assigned to PdBr2(dppe) VIII.
