Reaktion #169333
ord-dd4a7124c8dd49e49e889376485d2330
Reaktionsgleichung
Reagenzien
Reaktionsbedingungen
Temperatur
140°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeThe reaction mixture was evaporated in vacuo
- 2Extraktionthen extracted with DCM (3×20 mL)
- 3TrocknenThe combined organic extracts were dried over magnesium sulfate
- 4Sonstigeevaporated in vacuo
Vorschrift
Copper sulfate pentahydrate (55 mg, 0.24 mmol) was added to (5-bromopyridin-3-yl)(7-tert-butyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)methanone (292 mg, 0.81 mmol) (see Preparation 30) and concentrated ammonia solution (20 mL). The mixture was heated in a sealed vessel at 140° C. for 17 hours. The reaction mixture was evaporated in vacuo and the residue was stirred in aqueous hydrochloric acid (10 mL, 2M) at room temperature for 17 hours. The reaction mixture was basified to pH 9 using saturated aqueous sodium carbonate then extracted with DCM (3×20 mL). The combined organic extracts were dried over magnesium sulfate and evaporated in vacuo to afford the title compound as a white solid in 49% yield, 240 mg.