반응 #43414

ord-11ca716ac08e4600a5bb41b61801ea94

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도to reflux for 20 hours
  3. 3
    기타The cooled mixture was evaporated
  4. 4
    workup.ADDITIONthen diluted with water
  5. 5
    추출extracted with dichloromethane
  6. 6
    건조The organic extracts were dried over magnesium sulphate
  7. 7
    기타evaporated
  8. 8
    기타The residue was chromatographed on silica eluting with a gradient of 0-100% ethyl acetate in hexane affording product (168 mg, 65%)

실험 절차

A mixture of 8-[1-(chloromethyl)ethenyl]-3,7-difluoro-2-(methyloxy)-1,5-naphthyridine (320 mg, 1.18 mmol) and sodium iodide (885 mg) in acetonitrile (20 ml) was heated to reflux for 20 hours. The cooled mixture was evaporated then diluted with water and extracted with dichloromethane. The organic extracts were dried over magnesium sulphate and evaporated. The residue was chromatographed on silica eluting with a gradient of 0-100% ethyl acetate in hexane affording product (168 mg, 65%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07732460B2uspto-grants-2010_06