Optimization of the bromination reaction and conditions.
Entry | Condition | Time (min) | Yielda (%) |
---|---|---|---|
1b | Br2 (1 eq.), AcOH (1.2 eq.), ACN, rt | 60 | 36 |
2 | Br2 (3 eq.), ACH, 30 °C | 2 | 48 |
3 | Br2 (4.5 eq.), ACN, 30 °C | 2 | 22 |
4 | Br2 (3 eq.), ACN, 60 °C | 2 | 32 |
5 | Br2 (3 eq.), ACN, 30 °C | 4 | 28 |
6 | Br2 (3 eq.), MeOH, 30 °C | 2 | 44 |
7 | Br2 (3 eq.), ACN, 30 °C | 0.55 | 64 |
Isolated yield.
In a batch process.