反应详情

A mixture of (29) (2.52 g, 10 mmol)), N-chlorosuccinimide (1.6 g, 12 mmol), and benzoyl peroxide (1.21 g, 5 mmol) in carbon tetrachloride (50 ml) was refluxed for 2 hr. After cooling to room temperature, the mixture was filtered and the filtrate was evaporated in vacuo. The residue was purified by silica gel column chromatography (eluent, dichloromethane:EA (95:5)) to afford 493 mg (17%) of a yellow solid; 1H NMR (200 MHz, CDCl3) δ 2.63 (3H, s), 4.48 (2H, s), 7.27 (1H, s), 7.28 (1H, s), 7.76-7.98 (4H, m); m/z (EI) 286 (M+).

1. temperaturewas refluxed for 2 hr
2. filtrationthe mixture was filtered
3. customthe filtrate was evaporated in vacuo
4. customThe residue was purified by silica gel column chromatography (eluent, dichloromethane:EA (95:5))