반응 #48101

ord-1478545e3d4e4e06bc3aedf1e64970b7

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The solution is then cooled in an ice bath again
  2. 2
    기타At ambient temperature
  3. 3
    기타the organic phase is separated off
  4. 4
    추출the aqueous phase is extracted three times with ethyl acetate
  5. 5
    건조The combined organic phases are dried over sodium sulfate
  6. 6
    기타the solvent is removed completely

실험 절차

A solution of 14.8 g 1-bromo-4-chloro-3-(4-methoxy-benzyl)-benzene in 150 mL dichloromethane is cooled in an ice bath. 50 mL of a 1 M solution of boron tribromide in dichloromethane are added and the resulting solution is stirred for 2 h at ambient temperature. The solution is then cooled in an ice bath again and saturated aqueous potassium carbonate solution is added dropwise. At ambient temperature the mixture is adjusted with aqueous 1 M hydrochloric acid to pH 1, the organic phase is separated off and the aqueous phase is extracted three times with ethyl acetate. The combined organic phases are dried over sodium sulfate and the solvent is removed completely.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07745414B2uspto-grants-2010_06