反应详情

温度

60 °C

To a stirred mixture of 2,7-dibromofluorenone (26 g, 77 mmoles) and phenyl ether (170 g, 1 mole) is added 60 mL of methanesulfonic acid and 0.5 mL of 3-mercaptopropionic acid. The mixture is heated and stirred at 60° C. for 30 minutes, and then at 25° C. for 16 hours. The mixture is again stirred at 60° C. for 30 minutes and then at 25° C. for 3 hours. The mixture is poured into 1.4 L of ice water and 200 mL of methanol and allowed to stand in the hood for 4 days. The semi-solid precipitate is separated by decanting the supernatant liquid and then digesting with 1:1 v/v acetonitrile-hexane. The title compound is obtained as a colorless powder (32 g, 64 percent), melting point 178° C. to 180° C. HPLC analysis shows a purity of greater than 99 percent and the PMR spectrum (DMSO-d6) is consistent with the structure.

1. temperatureThe mixture is heated
2. waitat 25° C. for 16 hours
3. stirringThe mixture is again stirred at 60° C. for 30 minutes
4. waitat 25° C. for 3 hours
5. waitto stand in the hood for 4 days
6. customThe semi-solid precipitate is separated
7. customby decanting the supernatant liquid