Optimization of the ortho-C–H phosphorylation reaction conditions^a.

Entry	Deviation from standard conditions	Yield of 3ab(%)
1	None	73
2	H2O/CH3CN/TFE as solvent	−/−/65
3	Na2CO3/Na3PO4/NaOPiv as base	62/66/53
4c	Co(OAc)2·4H2O/Cu(OAc)2/Ni(DME)Cl2	Trace/0/0
5	N2 instead of air	72
6	Without electricity	0

^aReaction conditions A: undivided cell, GF anode, Pt cathode, 1a (0.3 mmol), 2a (4.0 equiv.), [Ru(OAc)₂(p-cymene)] (10 mol%), NaOAc (4.0 equiv.), HFIP: 1,1,1,3,3,3-hexafluoropropan-2-ol (3.0 mL), air, 65 °C, 3.5 mA, 24 h.

^bIsolated yields.

^cCo(OAc)₂·4H₂O (10 mol%)/Cu(OAc)₂ (10 mol%)/Ni(DME)Cl₂ (10 mol%).