Cycloaddition of carbon dioxide and epoxides over Fe-PYPA: Synthetic optimization and mechanistic study

From Alkenes to Cyclic Carbonates with a Stable Iron‐Cross‐Bridged Cyclam Catalyst

“…[44] Pyridine-based bidentate iron complex C8 combined with tetrabutylamonium iodide (TBAI) provided lower TOF than [Fe(L)Cl 2 ][PF 6 ] (entry 6 versus entry 10, Table 5) but it could be recycled for 6 cycles with a low decrease of conversion (5 %). [45] Tailor design of iron(III) aminophenolate catalyst provided examples with modest activity such as C9/TBAB (entries 7 and 8, Table 5) but introducing electron-withdrawing groups in the skeleton provided highly active catalytic systems combined with bis(triphenylphosphine)iminium chloride (PPNCl) (entry 9 versus entry 10, Table 5). [46] Regarding analogous cyclam-derived catalytic systems, there are few examples Reaction conditions: [a] Catalyst/Co-catalyst: 0.1/0.1 mol %; 100 °C, 20 bar, 4 h. [b] Catalyst/Co-catalyst: 0.1/0.1 mol %; 130 °C, 40 bar, 4 h. [c] Catalyst/ Co-catalyst: 0.2/0.2 mol %; 100 °C, 40 bar, 12 h. [d] Catalyst/Co-catalyst: 0.5/-mol %; 80 °C, 35 bar, 20 h, TOF estimated from data reported.…”

Application ofin situATR-IR spectroscopy for the synthesis of bisphenol F: optimization, mechanistic and kinetics studies

“…31 Crucial reaction intermediates in the synthesis of benzoxazole were observed with ATR-IR spectroscopy integrated with a flow cell coupled with a nuclear magnetic resonance (NMR) spectrometer. 34 Recently, we used ATR-IR spectroscopy to trace the synthetic process and reaction mechanism in important CO 2 cycloadditions 35 and production of key pharmaceutical intermediates. 36 Conversely, Raman spectroscopy is a very good adjunct to ATR-IR spectroscopy in reaction monitoring and mechanistic studies.…”