반응 #156669

ord-66c2ac52b43d4554bf0846769ba756fa

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Then the ice bath was removed
  2. 2
    온도Then the mixture was cooled to 0° C.
  3. 3
    workup.ADDITIONwater was added
  4. 4
    추출the aqueous phase was extracted several times with ethyl acetate
  5. 5
    건조dried over sodium sulfate
  6. 6
    기타the solvent was removed in vacuum
  7. 7
    기타In this way the product was obtained with molecular weight 162.03 (C9H6O3)

실험 절차

A 1M solution of boron tribromide in methylene chloride (101 mL) was added at 0° C. to a solution of 6-methoxy-isochromen-1-one (8.9 g) in methylene chloride (178 mL). Then the ice bath was removed and the reaction mixture was stirred overnight at room temperature. Then the mixture was cooled to 0° C., water was added and the aqueous phase was extracted several times with ethyl acetate. The organic phases were combined, dried over sodium sulfate and the solvent was removed in vacuum. In this way the product was obtained with molecular weight 162.03 (C9H6O3); MS (ESI): 163 (M+H+).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08822495B2uspto-grants-2014_09