反応 #47079

ord-5225d5b0cbab47c99e8ebeaf194f62e9

溶媒

反応条件

温度
50°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture is cooled to RT
  2. 2
    洗浄washed with water, brine
  3. 3
    乾燥dried (MgSO4)
  4. 4
    ろ過filtered
  5. 5
    その他The filtrate is evaporated
  6. 6
    その他the residue purified by chromatography on silica gel
  7. 7
    洗浄elution with dichloromethane

実験手順

To a solution of 4-fluorophenol (560 mg, 5.0 mmol) in DMF (10 mL) is added potassium carbonate (828 mg, 6.0 mmol) followed by chloroacetonitrile (0.315 mL, 50.0 mmol). The reaction mixture is stirred and heated at 50° C. for 14 h. The reaction mixture is cooled to RT, diluted with EtOAc, and washed with water, brine, then dried (MgSO4), and filtered. The filtrate is evaporated, and the residue purified by chromatography on silica gel; elution with dichloromethane gives 721 mg of the product 388.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07741493B2uspto-grants-2010_06