Table 1.
Entry | Deviation from Standard Conditions | Yield (%) | ir (3a:3b) |
---|---|---|---|
1 | none | 64 | 1:1.4 |
2 | 60 °C | 65 | 1:4 |
3 | 60 °C, 0.1 M | 67 | 1:10 |
4 | added LiCl (62.5 mol%) | 52 | 1:1 |
5 | 0% FeCl3 | 0 | - |
6 | in the dark | 0 | - |
7 | irradiate at 390 nm 1 h, then dark | 2 | n.d. |
8 | 427 nm LED | 3 | n.d. |
9 | under air | 47 | 1:1 |
Reactions were performed on a 0.3 mmol scale. Yields were determined by 1H NMR using 1,3,5-trimethoxybenzene as the internal standard. n.d.: not determined.