反应详情

A solution of 31.9 g (0.1 mol) of 7-(4-bromo-2,5-difluorophenyl)-1,4-dioxaspiro[4.4]nonane in 300 ml of dry tetrahydrofuran, under an argon atmosphere at -78° C., was treated with 40 ml (0.1 mol) of 2.5 M n-butyl lithium (hexane solution). The solution was warmed to -40° and poured onto 500 g of finely crushed dry ice and the mixture allowed to stand until the dry ice evaporated (18 hours). The solvent was evaporated in vacuo and the residue partitioned between ethyl acetate/1.0 M hydrochloric acid (500 ml ea). The organic layer was washed with water, dried (MgSO4), and evaporated in vacuo to give 18.9 g of the title compound.

1. temperatureThe solution was warmed to -40°
2. customevaporated (18 hours)
3. customThe solvent was evaporated in vacuo
4. customthe residue partitioned between ethyl acetate/1.0 M hydrochloric acid (500 ml ea)
5. washThe organic layer was washed with water
6. dry with materialdried (MgSO4)
7. customevaporated in vacuo