反応 #52471

ord-bd72d4cb452c487da230242602390675

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with EtOAc
  2. 2
    洗浄The combined organic layers were washed with H2O and saturated aqueous NaCl
  3. 3
    乾燥before being dried (MgSO4)
  4. 4
    濃縮concentrated under reduced pressure

実験手順

To a solution of 4-bromo-3-tert-butylphenol (Intermediate 104, 1.17 g, 5.10 mmols) and imidazole (520.0 mg, 7.65 mmols) in 10 mL DMF was added chloro-triisopropylsilane (1.18 g, 6.10 mmols). After stirring overnight at room temperature the solution was diluted with H2O and extracted with EtOAc. The combined organic layers were washed with H2O and saturated aqueous NaCl before being dried (MgSO4) and concentrated under reduced pressure. The title compound, 1.80 g (92%), was isolated by column chromatography (0-1.5% EtOAc—hexanes) as a colorless oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06855512B2uspto-grants-2005_02