反应详情

A solution of the 4'-chloro-4-chloropropoxybenzophenone (3.0 g, 9.7 mmol) and imidazole (1.3 g, 19 mmol) in 2-methoxyethyl ether (20 mL) was heated to 120° C. for 24 hours. The solvent was removed by distillation and the resulting residue was chromatographed (flash, SiGel, 9:1 CH2Cl2 -MeOH). The hydrochloride salt was made in HCl/MeOH and recrystallized from acetone to give 1.2 g (36%) of the title compound as a white solid. m.p. 210°-212° C. IR (KBr): 1645, 1601cm-1. MS: 341 (MH) . 1H NMR (CD3OD): δ9.00(s,1H), 7.89-6.87(m,10H), 4.11(t,2H), 3.45(t,2H), 2.11(m,2H).

1. customThe solvent was removed by distillation
2. customthe resulting residue was chromatographed (flash, SiGel, 9:1 CH2Cl2 -MeOH)
3. customrecrystallized from acetone