反応 #2032490

ord-6cdfe8153d384caf93eb044a18277248

溶媒

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGThe reaction was stirred at rt for 1 h
  2. 2
    その他partitioned between water and EtOAc
  3. 3
    抽出The aqueous layer was extracted with EtOAc
  4. 4
    洗浄the combined organic layers were washed with brine
  5. 5
    乾燥dried (Na2SO4)
  6. 6
    ろ過filtered
  7. 7
    濃縮concentrated
  8. 8
    その他The crude product was used in the next step without further purification

実験手順

NaH (81 mg, 3.21 mmol) was added to a 0° C. solution of 5-bromo-6-fluoro-1H-indole (0.343 g, 1.60 mmol) in THF (16 mL). The reaction mixture was stirred at 0° C. for 15 min, then ethyl bromoacetate (0.535 mL, 4.81 mmol) was added. The reaction was stirred at rt for 1 h, then partitioned between water and EtOAc. The aqueous layer was extracted with EtOAc and the combined organic layers were washed with brine, dried (Na2SO4), filtered, and concentrated. The crude product was used in the next step without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08394969B2uspto-grants-2013_03