반응 #169333

ord-dd4a7124c8dd49e49e889376485d2330

반응 조건

온도
140°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction mixture was evaporated in vacuo
  2. 2
    추출then extracted with DCM (3×20 mL)
  3. 3
    건조The combined organic extracts were dried over magnesium sulfate
  4. 4
    기타evaporated 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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846698B2uspto-grants-2014_09