反应详情

4.6 g (15 mmol) of di(1-adamantyl)phosphine were placed in 50 ml of di-n-butyl ether, and 20 ml of a 2.5 M solution of n-BuLi in toluene (50 mmol) were added. The mixture was refluxed for 1 h and cooled and 4.1 g (30 mmol) of 1-butyl bromide were added dropwise. The mixture was refluxed for 30 min, cooled and washed with saturated ammonium chloride solution (3×), the organic phase was separated off and dried over sodium sulfate and the solvent was distilled off under reduced pressure.

1. temperatureThe mixture was refluxed for 1 h
2. temperaturecooled
3. temperatureThe mixture was refluxed for 30 min
4. temperaturecooled
5. washwashed with saturated ammonium chloride solution (3×)
6. customthe organic phase was separated off
7. dry with materialdried over sodium sulfate
8. distillationthe solvent was distilled off under reduced pressure