反应详情

(2-Amino-5-bromo-phenyl)-phenyl-methanone (10 g, 36 mmol), methanesulfonylacetone (7.4 g, 54 mmol) and sodium tetrachloroaureate(III) dihydrate (720 mg, 1.8 mmol) were heated at reflux in 2-propanol (100 mL) for 4.5 days. The resulting suspension was evaporated to dryness and the residue extracted with dichloromethane (2×), 1 N NaOH (2×), which removes excess of methanesulfonylacetone, and sat. NaCl (1×). The crude product was purified twice by chromatography in dichloromethane and then crystallized from dichloromethane/heptane by evaporation of dichloromethane. One obtained 4.6 g (33%) of beige crystals. MS: m/z=375/377 (M).

1. customThe resulting suspension was evaporated to dryness
2. extractionthe residue extracted with dichloromethane (2×), 1 N NaOH (2×), which
3. customremoves excess of methanesulfonylacetone, and sat. NaCl (1×)
4. customThe crude product was purified twice by chromatography in dichloromethane
5. customcrystallized from dichloromethane/heptane by evaporation of dichloromethane