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. 2022 Feb 14;2(3):731–744. doi: 10.1021/jacsau.2c00005

Table 2. Treatment of CuI, NaBPh4, and L1 with CO2 under Varying Reactions Conditionsa.

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entry CuI [μmol] parameter t [h] 13C NMR (C2O42–) CE (C2O42– (?)) [%]b
1 120 - 24 n.d. <1
2 120 - 118 n.d. <0.5
3 182 - 120 n.d. <0.5
4 120 MeOH/THF (9:1) 118 n.d. <0.5
5 124 THF 120 n.d. <0.5
6 123 toluene 121 n.d. <1
7 120 40 °C 114 n.d. 3
8 122 40 °C 123 n.d. 8
9 133 400–700 nm (0.09 W) 18 n.d. <0.5
10 130 10 bar 116 n.d. 16
11 132 10 bar 116 n.d. 12
a

Reaction conditions: CuI/L1/NaBPh4 (1:1:1) was utilized in degassed MeOH under constant CO2 atmosphere, unless indicated by the varied parameter. n.d. = not detected.

b

Oxalate yields were calculated for signals coinciding with Na2C2O4 added as internal standard after initial measurement and were found to overlap with the signal of iodide.