반응 #1851983

ord-58be4f3deb1344229084f288ffb32d2e

반응 조건

온도
130°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was cooled
  2. 2
    workup.STIRRINGAfter stirring for 10 minutes
  3. 3
    추출the water mixture was extracted with ether (3×100 mL)
  4. 4
    세척The ether layer was washed with brine (100 mL)
  5. 5
    건조dried over MgSO4
  6. 6
    여과filtered
  7. 7
    농축concentrated to a residue

실험 절차

To a cold boron trifluoride etherate (280 mmol) solution was added 3-fluorophenol or phenol (89 mmol) and 4-chlorobutyryl chloride (178 mmol). The resulting solution was stirred at 130° C. for 18 hours. The reaction mixture was cooled and poured into ice water (100 mL). After stirring for 10 minutes, the water mixture was extracted with ether (3×100 mL). The ether layer was washed with brine (100 mL), dried over MgSO4, filtered and concentrated to a residue to afford 4-chloro-1-(4-fluoro-2-hydroxyphenyl)butan-1-one and 4-chloro-1-(2-hydroxyphenyl)butan-1-one in 52%-67% yield, which was used in the following step without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE039680E1uspto-grants-2007_06