反応 #48101

ord-1478545e3d4e4e06bc3aedf1e64970b7

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The solution is then cooled in an ice bath again
  2. 2
    その他At ambient temperature
  3. 3
    その他the organic phase is separated off
  4. 4
    抽出the aqueous phase is extracted three times with ethyl acetate
  5. 5
    乾燥The combined organic phases are dried over sodium sulfate
  6. 6
    その他the solvent is removed completely

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07745414B2uspto-grants-2010_06