反応 #53056

ord-1e02debe0c2c40d8bd1bb285536265c9

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度refluxed for 60 minutes
  2. 2
    濃縮The solvent is concentrated by evaporation
  3. 3
    温度refluxed for 90 minutes
  4. 4
    ろ過filtered
  5. 5
    洗浄washed with methanol
  6. 6
    その他dried

実験手順

390 mg (0.7 mmol) of (Z)-3-{1-[4-(N—(N-benzylpiperazinomethylcarbonyl)-N-methylamino)-phenylamino]-1-phenyl-methylidene}-2-indolinone are dissolved in 20 ml of dichloromethane and after the addition of 0.2 g (1.4 mmol) of 1-chloroethyl chloroformate heated for 30 minutes at ambient temperature and refluxed for 60 minutes. The solvent is concentrated by evaporation, the residue is combined with 10 ml of methanol and refluxed for 90 minutes. After 18 hours stirring at ambient temperature, the product is suction filtered, washed with methanol and dried.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06855710B2uspto-grants-2005_02