反应详情

温度

-30 °C

Next, 5.0 g (17.5 millimole) of 2-bromo-4,6-di-tert-butylphenol described above was dissolved in 45 ml of dehydrated diethyl ether under nitrogen flow, and the solution was cooled down to −30° C. Then, 23.3 ml (37.3 millimole) of a hexane solution having an n-butyllithium concentration of 1.6 mole/liter was added thereto, and then the solution was stirred at a room temperature for 5 hours. The reaction mixture was cooled down to −30° C., and 3.26 ml (17.3 millimole) of diphenylchlorophosphine was added thereto and stirred at a room temperature for 8 hours. In this reaction solution, 2.6 ml (20.5 millimole) of trimethylsilyl chloride was added, and the solution was further stirred for 8 hours. Then, the solvent was distilled off under reduced pressure, and the residue was extracted with hexane. Subsequently, after the solvent was distilled off under reduced pressure, the residue was dissolved in hexane, and the solution was then cooled down to separate a precipitated solid matter, whereby 1.3 g (yield: 16%) of 4,6-di-tert-butyl-2-diphenylphosphinophenyl trimethylsilyl ether was obtained.

1. additionwas added
2. temperatureThe reaction mixture was cooled down to −30° C.
3. stirringstirred at a room temperature for 8 hours
4. stirringthe solution was further stirred for 8 hours
5. distillationThen, the solvent was distilled off under reduced pressure
6. extractionthe residue was extracted with hexane
7. distillationSubsequently, after the solvent was distilled off under reduced pressure
8. dissolutionthe residue was dissolved in hexane
9. temperaturethe solution was then cooled down
10. customto separate a precipitated solid matter