反应详情

温度

210 °C

A mixture of 4-bromoanisole (35 ml, 0.28 mol), 4-chlorophenol (43 g, 0.33 mol), anhydrous K2CO3 (13 g, 0.09 mol) and copper bronze (0.38 g, 5.98 mmol) were stirred under a nitrogen atmosphere at 210° C. for 2 hours. After cooling to room temperature, the mixture was dissolved in methylene chloride, extracted two times with 1 N NaOH, dried (MgSO4) and the solvent removed under reduced pressure to give a brown liquid. Excess 4-bromoanisole was removed by distillation under reduced pressure (60°-73° C., 1 mm) and the residual crystalline solid was purified by HPLC (hexane-methylene chloride). 4-Methoxy-4'-chlorodiphenyl ether was isolated as a white crystalline solid (28.84 g, 44%), mp 49°-51° C.

1. temperatureAfter cooling to room temperature
2. extractionextracted two times with 1 N NaOH
3. dry with materialdried (MgSO4)
4. customthe solvent removed under reduced pressure
5. customto give a brown liquid
6. customExcess 4-bromoanisole was removed by distillation under reduced pressure (60°-73° C., 1 mm)
7. customthe residual crystalline solid was purified by HPLC (hexane-methylene chloride)