反应详情

nButyllithium (12.2 mL, 30.6 mmol, 2.5 M in hexanes) was added to toluene-4-sulfonic acid 2-(4-chloro-pyrrolo[2,3-d]pyrimidin-7-yl)-3-hydroxy-2-hydroxymethyl-propyl ester (Preparation 210, 5.73 g, 13.9 mmol) in THF (100 mL) at 0° C. and stirred for 5 min. The reaction mixture was then warmed to room temperature and stirred for 16 hours, at which point it was quenched with saturated aqueous ammonium chloride. The resulting mixture was extracted with ethyl acetate (100 mL×3) and the combined organic phases were dried (MgSO4) and concentrated in vacuo. The crude product was triturated with dichloromethane and filtered to afford the title compound in 36% yield, 1.2 g.

1. stirringstirred for 16 hours, at which point it
2. customwas quenched with saturated aqueous ammonium chloride
3. extractionThe resulting mixture was extracted with ethyl acetate (100 mL×3)
4. dry with materialthe combined organic phases were dried (MgSO4)
5. concentrationconcentrated in vacuo
6. customThe crude product was triturated with dichloromethane
7. filtrationfiltered