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. Author manuscript; available in PMC: 2020 Jul 30.
Published in final edited form as: J Am Chem Soc. 2020 Mar 10;142(12):5568–5573. doi: 10.1021/jacs.0c02441

Table 1.

Selected Optimization Studies

graphic file with name nihms-1611977-t0005.jpg
entry solvent catalyst (mol %) temp (°C) yield (%)a notes
1 CH2CI2 Rh2(TPA)4 (1) rt 24 15% rsm
2 CH2Cl2 (0.2 M) Rh2(TPA)4 (1) rt 28 –
3 CH2Cl2 (0.05 M) Rh2(TPA)4 (1) rt 33 –
4 CH2Q2 Rh2(TPA)4 (1) 50 41 –
5 CH2Q2 Rh2(TPA)4 (1) 50 33 catalyst added last
6 CH2Q2 Rh2(TPA)4 (1) 50 21 PhI(OAc)2
7 MeNO2 Rh2(TPA)4 (1) 45 23 –
8 CH2CI2 Rh2(TPA)4 (5) 50 55 LUMO = −2.90 eV
9 CH2CI2 Rh2(TPA)4 (5) 50 58 0.05 equiv of PhIO × 3, added every 20 min
10 CICH2CH2CI Rh2(TPA)4 (5) 80 49 –
11 CH2CI2 Rh2(OAc)4 (5) 50 42 LUMO = −2.68 eV
12 CH2CI2 Rh2(esp)2 (5) 50 41 LUMO = −2.71 eV
a

NMR yields using mesitylene as an internal standard.