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. Author manuscript; available in PMC: 2021 Aug 21.
Published in final edited form as: J Org Chem. 2020 Aug 5;85(16):10451–10465. doi: 10.1021/acs.joc.0c00415

Figure 3:

Figure 3:

10 K EPR Analysis of Co Catalytic Center. Reaction Conditions: [A] Co(acac)2 (1.0 equiv., 0.10 mmol) was stirred in 0.40 mL of DCB at 90 °C in Ar for 15 min. A 100 μL sample was quenched in N2(l) (left). Then Ar was exchanged for O2 and reacted at 90 °C for 2 h. A 100 μL sample was quenched in N2(l) (right). [B] 4a (1.0 equiv., 0.10 mmol) was reacted with Co(acac)2 (1.0 equiv., 0.10 mmol) in 0.40 mL of DCB at 90 °C in Ar for 15 min. A 100 μL sample was quenched in N2(l) (left). Then Ar was exchanged for O2 and reacted at 90 °C for 2 h. A 100 μL sample was quenched in N2(l) (right). [C] 2 (3.0 equiv., 0.30 mmol) was stirred in the presence of Co(acac)2 (1.0 equiv., 0.10 mmol) in 0.40 mL of DCB at 90 °C in Ar for 15 min. A 100 μL sample was quenched in N2(l) (left). Then Ar was exchanged for O2 and reacted at 90 °C for 2 h. A 100 μL sample was quenched in N2(l) a (right). [D] 4a (1.0 equiv., 0.10 mmol) was reacted with 2 (3.0 equiv., 0.30 mmol) in the presence of Co(acac)2 (0.10 equiv., 0.010 mmol) in 0.40 mL of DCB at 90 °C in Ar for 15 min. A 100 μL sample was quenched in N2(l) (left). Then Ar was exchanged for O2 and reacted at 90 °C for 2 h. A 100 μL sample was quenched in N2(l) (right). [E] Calculated spectra using the EasySpin toolbox from Matlab27 for Co(acac)2(EtOH)2.28