Optimization with respect to NBSa.
Entry | Solventb | Reactant 1 (equivalent) | NBS (equivalent) | Photon flux (μmol s−1) | Time (h) | Yieldc (%) |
---|---|---|---|---|---|---|
1 | CH3CN | 1 | 1.05 | 21 | 10 | 48* |
2 | CH3CN | 1 | 1.3 | 21 | 10 | 55* |
3 | CH3CN | 1 | 1.5 | 21 | 10 | 67* |
4 | CH3CN | 1 | 1.8 | 21 | 10 | 73* |
5 | CH3CN | 1 | 2.0 | 21 | 10 | 77* |
6 | CH3CN | 1 | 2.2 | 21 | 5 | 84 |
Reaction condition: 1 (0.6 mmol) and NBS were taken in acetonitrile.
Volume of solvent: 1 mL.
Pure product was isolated by silica-gel column chromatography, * starting material was not consumed.