反应详情

nBuLi (20 cm3, 32 mmol 1.6M soln) was added over 1 hour to a cooled solution of 1-adamantyl phosphine (5.0 g, 30 mmol) in THF (100 cm3). The solution was allowed to warm to room temperature and stirred for a further 2 hours. The solution was recooled to 0° C. and tert-butylchloride (2.78 g, 30 mmol) was added and stirring continued for a further 16 hours at room temperature. The reaction mixture was quenched with water and the aqueous phase extracted with dichloromethane (2×50 ml). The organic phase was dried over sodium sulphate and evaporated in-vacuo to yield the title compound.

1. customwas recooled to 0° C.
2. stirringstirring
3. waitcontinued for a further 16 hours at room temperature
4. customThe reaction mixture was quenched with water
5. extractionthe aqueous phase extracted with dichloromethane (2×50 ml)
6. dry with materialThe organic phase was dried over sodium sulphate
7. customevaporated in-vacuo