반응 #53056

ord-1e02debe0c2c40d8bd1bb285536265c9

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed for 60 minutes
  2. 2
    농축The solvent is concentrated by evaporation
  3. 3
    온도refluxed for 90 minutes
  4. 4
    여과filtered
  5. 5
    세척washed with methanol
  6. 6
    기타dried

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06855710B2uspto-grants-2005_02