反应详情

To a solution of dibenzothiophen-4-ol (i)(14.2 g, 71.0 mmol) in acetone (500 ml) was added powdered potassium carbonate (14.72 g, 106.5 mmol) and methyl iodide (4.43 ml, 71 mmol). The mixture was heated to reflux and stirred like this for 16 hours. The mixture was then cooled and filtered through a Celite™ pad. The resulting filtrant was concentrated in vacuo to give an oily residue that was diluted in dichloromethane (100 ml) and washed with 1M NaOH and saturated brine solution. The organic layer was dried using MgSO4, filtered and concentrated in vacuo to give a buff coloured solid that corresponded to the title compound and was used without any further purification. (15.2 g, 100%) m/z (LC-MS, ESP), RT=4.22 min, (M+H)=215.1.

1. temperatureThe mixture was heated
2. temperatureto reflux
3. temperatureThe mixture was then cooled
4. filtrationfiltered through a Celite™ pad
5. concentrationThe resulting filtrant was concentrated in vacuo
6. customto give an oily residue that
7. washwashed with 1M NaOH and saturated brine solution
8. customThe organic layer was dried
9. filtrationfiltered
10. concentrationconcentrated in vacuo
11. customto give a buff