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. Author manuscript; available in PMC: 2023 Mar 2.
Published in final edited form as: J Am Chem Soc. 2022 Feb 21;144(8):3353–3359. doi: 10.1021/jacs.1c13299

Table 1.

Selected Optimization Experiments.a

graphic file with name nihms-1790325-t0002.jpg
Entry Deviation from the standard conditions Yield (%) ax:eq
1 none 83 4.2:1
2 Pd(OAc)2 instead of Pd(PPh3)4 19 4.8:1
3 no Pd(PPh3)4 <2 -
4 Ru(bpy)3(PF6)2 <2 -
5 Ir(PPy)2(dtbbpy)PF6 <2 -
6 no Xantphos 30 4.2:1
7 DIPEA instead of K3PO4 52 4.2:1
8 Cs2CO3 instead of K3PO4 67 4.2:1
9 no Base 8 4.2:1
10 room temperature <2 -
11 with air <2 -
12 no light <2 -
a

See the Supporting Information (SI) for experimental details. Yields of 3a and axial:equatorial (ax:eq) ratios were determined by 1H NMR analysis using dibromomethane as the internal standard.