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. 2019 May 8;21(10):3764–3768. doi: 10.1021/acs.orglett.9b01205

Table 1. Effect of Deviation from Standard Reaction Conditionsa.

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entry variation from standard conditions yieldb (%)
1 none 83 (82)c
2 no light 0
3 air atmosphere 28
4 no photocatalyst 0
5 0.5% [Ru] loading 52
6 (Ir[dF(CF3)ppy]2(dtbbpy))PF6 (1 mol %) 28
7 [Ir(dtbbpy)(ppy)2]PF6 (1 mol %) 16
8 no AscH2 0
9 AscH2 (2 equiv) 18
10 AscH2 (3 equiv) 79
11 Na-ascorbate instead of AscH2 0
12 30 min reaction time 36
13 MeOH 29
14 MeOH/H2O (10:1) 41
15 MeOH/H2O (6:1) 62
16 MeOH/H2O (2:1) 71
17 EtOH/H2O (1:1) 81
18 AcOH additive (10 vol %) 58
19 DMF 11
20 MeCN 0
a

Full reaction optimization in Tables S1–S7.

b

GC yield: average of two runs.

c

Isolated yield by SiO2 column chromatography