反应详情

9-Methylfluorene (43.6 g, 0.24 mol) and N-chlorosuccinimide (64.5 g, 0.48 mol) were suspended in 25 mL of acetonitrile and cooled in an ice-water bath. Then 20 mL of concentrated HCl was added dropwise and the solution was stirred at room temperature overnight. The precipitate was filtered and dried. Recrystallization from EtOH and water gave 24 g (41%) of 2,7-dichloro-9-methylfluorene as white crystals, mp 110°-112° C. FT IR: 3425, 1450, 1407, 1273, 1167, 1070, 851,818 cm-1 ; H1NMR (CDCl3, 300 MHz) δ 7.3-7.8 (m, 6H, 3.9-4.1 (q, 1H), 1.2-1.3 (d, 2H).

1. temperaturecooled in an ice-water bath
2. filtrationThe precipitate was filtered
3. customdried
4. customRecrystallization from EtOH and water