反应详情

To a suspension of sodium hydride (7.28 mmol, 10 equiv.) in tetrahydrofuran (10 ml) there was added, at 0° C., N-cyclopropyl-N-(2-hydroxyethyl)-4-methoxy-2,6-dimethylphenylsulfonamide (C-10) (0.8 mmol, 1.1 equiv.), followed by 3-(6-chloro-pyrimidin-4-yl)-9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane (0.73 mmol, 1 equiv.). The reaction mixture was stirrred overnight at room temperature; water was then added and the mixture was diluted with ethyl acetate. The organic phase was extracted with water and saturated sodium chloride solution, dried (Na2SO4) and concentrated in vacuo. The crude product was purified by column chromatography (Alox-neutral). Yield: 7%. Rt=3.4 min; m/z=607.5 [MH]+

1. additionwas added, at 0° C.
2. extractionThe organic phase was extracted with water and saturated sodium chloride solution
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated in vacuo
5. customThe crude product was purified by column chromatography (Alox-neutral)