Optimisation and control experimentsab.
Entry | Light | Additive (1.0 equiv.) | Temp. [°C] | Yield [%] |
---|---|---|---|---|
1 | 15 W blue LEDs (448 nm) | — | R.T. | 55 (54)c |
2 | Dark | — | R.T. | N. D. |
3 | Dark | — | 65 | N. D. |
4 | 15 W green LEDs (530 nm) | — | R.T. | 6 |
5 | 15 W blue LEDs (448 nm) | Run with 2 equiv. of CF3(CF2)3I | R.T. | 50 |
6 | 15 W blue LEDs (448 nm) | Oxone | R.T. | 89c |
7d | 15 W blue LEDs (448 nm) | Oxone | R.T. | 77c |
8 | 15 W blue LEDs (448 nm) | K2S2O8 | R.T. | 58 |
9 | 15 W blue LEDs (448 nm) | (NH4)2S2O8 | R.T. | 50 |
10 | 15 W blue LEDs (448 nm) | PhI(OAc)2 | R.T. | N. D. |
11 | 15 W blue LEDs (448 nm) | [FeCp2]PF6 | R.T. | 86c |
12 | 15 W blue LEDs (448 nm) | AgOAc | R.T. | 33 |
General conditions: palladacycle 1 (1.0 equiv.), CF3(CF2)3I (2) (1 equiv.), solvent (0.1 M in substrate), 16 h.
Yield determined by 1H NMR spectroscopy using 2,5-dimethylfuran as an internal standard.
Isolated yield.
Under air.