反应详情

5.5 g (18 mmol) of di(1-adamantyl)phosphine were placed in 60 ml of di-n-butyl ether, and 20 ml of a 2.5 M solution of n-BuLi (50 mmol) in toluene were added. The mixture was refluxed for 45 min and cooled and 3.0 g (18 mmol) of 1-bromohexane 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 45 min
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