反応 #53331

ord-46fa65e8e380434ab77bc22111932839

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGthe reaction mixture was stirred at RT for 16 hours
  2. 2
    その他The reaction mixture was quenched with H2O
  3. 3
    workup.STIRRINGstirred
  4. 4
    ろ過The resulting precipitate was filtered off
  5. 5
    workup.STIRRINGthe residue was stirred
  6. 6
    温度in refluxing methanol
  7. 7
    温度cooled
  8. 8
    ろ過filtered

実験手順

NaOH (0.0128 mol), 1,4-dioxane (5 ml), and guanidine (0.0128 mol) were combined and stirred at RT for 5 minutes under argon. Then, intermediate (27) (0.00128 mol) was added and the reaction mixture was stirred at RT for 16 hours. The reaction mixture was quenched with H2O, and stirred. The resulting precipitate was filtered off and the residue was stirred in refluxing methanol, cooled, and filtered, yielding 0.34 g (64.3%) of N-[4-[(4-cyanophenyl)amino]-6-[(2,6-dichlorophenyl)methyl]-1,3,5-triazin-2-yl]-guanidine (compound 20).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06858609B2uspto-grants-2005_02