Table 1.
Entry | Variation of standard conditions | Yield (%)b |
---|---|---|
1 | None | 92 (91c) |
2 | L2 instead of L1 | 37 |
3 | L3 instead of L1 | 66 |
4 | L4 instead of L1 | 63 |
5 | L5 instead of L1 | 27 |
6 | FeCl3 instead of FeI2 | 7 |
7 | Fe(acac)3 instead of FeI2 | nd |
8 | PhSiH3 instead of (EtO)3SiH | 79 |
9 | Without 4CzIPN | 59 (88d) |
10 | Without FeI2 | nd |
11 | Without light irradiation | nd |
nd not detected, blue LED blue light-emitting diode.
aStandard conditions: 4CzIPN (1 mol%), FeI2 (10 mol%), L1 (10 mol%), 1 (0.6 mmol), 2 (0.2 mmol), 2,6-lutidine (3.0 equiv.), (EtO)3SiH (2.0 equiv.), MeCN (2 mL), blue LEDs, 65 °C, 24 h.
bGC yield. cIsolated yield.
dTime = 44 h. See Supplementary Information for additional optimization experiments.