反应详情

A mixture of 2,6-dibromophenol (25 g, 0.099 mol), powder potassium carbonate (28 g, 0.2 mol, 2 equiv) and dimethyl sulfate (12.6 g, 0.099 mol) in acetonitrile (400 mL) was kept at reflux with good stirring for 4 hr. After cooling, the solids were removed by filtration and the solvent was removed in a rotary evaporator. The residue was taken in 2:1 heptane/ethyl acetate mixture (800 mL) and washed with water (2×400 mL). The organic layer was dried over sodium sulfate, filtered and the solvent was removed in a rotary evaporator, leaving almost pure 1 (15.5 g, 96%).

1. temperatureat reflux
2. temperatureAfter cooling
3. customthe solids were removed by filtration
4. customthe solvent was removed in a rotary evaporator
5. washwashed with water (2×400 mL)
6. dry with materialThe organic layer was dried over sodium sulfate
7. filtrationfiltered
8. customthe solvent was removed in a rotary evaporator