反应详情

A stirred solution of 4-(5-phenyl-2-thienyl)-2-naphthol, (0.52 g, 1.73 mmol) and 1-(2-fluorophenyl)-1-(4-pyrrolidinophenyl)prop-2-yn-1-ol (0.51 g, 1.73 mmol) in toluene (50 ml) was warmed to 50° C. Acidic Al2O3 (1 g) was then added and the mixture heated to reflux for 1.5 h. After cooling, the solution was filtered, washed with hot toluene (100 ml) and the solvent removed. The resulting residue was then flash chromatographed eluting with EtOAc-hexane (1:9). The fractions were combined and the solvent removed. After precipitation from acetone-MeOH, the title compound (0.52 g, 52%) was collected as dark green crystals.

1. temperaturethe mixture heated
2. temperatureto reflux for 1.5 h
3. temperatureAfter cooling
4. filtrationthe solution was filtered
5. washwashed with hot toluene (100 ml)
6. customthe solvent removed
7. customflash chromatographed
8. washeluting with EtOAc-hexane (1:9)
9. customthe solvent removed
10. customAfter precipitation from acetone-MeOH
11. customthe title compound (0.52 g, 52%) was collected as dark green crystals