反应详情

温度

0 °C

7.40 g (23.4 mmol) of 1,3-difluoro-5-hydroxymethyl-2-triisopropylsilanyloxybenzene are dissolved in 90 ml of dry dichloromethane by stirring at 0° C. under argon. 10.1 g (30.4 mmol) of tetrabromomethane and 7.97 g (30.4 mmol) of triphenylphosphine are successively added to this solution, and the mixture is then stirred under reflux under argon for 12 h. The reaction mixture is washed with water, the organic phase is separated off, dried over magnesium sulfate and filtered, and the solvent is distilled out in vacuo. The oily residue is taken up in diethyl ether and stirred at RT, then filtered, and the filtrate is concentrated. Chromatography of the residue on silica gel 60 (mobile phase: cyclohexane/ethyl acetate 9:1) results in 7.42 g (15.6 mmol, 84% of theory) of the title compound.

1. stirringthe mixture is then stirred
2. temperatureunder reflux under argon for 12 h
3. washThe reaction mixture is washed with water
4. customthe organic phase is separated off
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. distillationthe solvent is distilled out in vacuo
8. stirringstirred at RT
9. filtrationfiltered
10. concentrationthe filtrate is concentrated