반응 #169333
ord-dd4a7124c8dd49e49e889376485d2330
반응 방정식
반응 조건
온도
140°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타The reaction mixture was evaporated in vacuo
- 2추출then extracted with DCM (3×20 mL)
- 3건조The combined organic extracts were dried over magnesium sulfate
- 4기타evaporated in vacuo
실험 절차
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.