反应详情

A solution of Dibenzo[b,d]furan-4-ol (1 g, 5.43 mmol) in DMF (5 ml) was added to a stirred and cooled (0° C.) suspension of 60% sodium hydride (326 mg, 8.12 mmol) in DMF (20 ml). The mixture was stirred at 0° C. for 5 min and ethyl iodide (1.18 g, 10.86 mmol) in DMF (5 ml) was added dropwise over a period of 10 min. The cooling bath was removed and the mixture was stirred for 1 h at room temperature. The reaction mixture was diluted with ice-cold water (100 ml) and extracted with EtOAc (3×50 ml). The combined organic extracts were washed with water (2×100 ml), brine (100 ml) and dried (Na2SO4), to give 0.95 g (82%) of the product as viscous liquid,

1. temperaturecooled
2. stirringThe mixture was stirred at 0° C. for 5 min
3. customThe cooling bath was removed
4. stirringthe mixture was stirred for 1 h at room temperature
5. additionThe reaction mixture was diluted with ice-cold water (100 ml)
6. extractionextracted with EtOAc (3×50 ml)
7. washThe combined organic extracts were washed with water (2×100 ml), brine (100 ml)
8. dry with materialdried (Na2SO4)