تفاعل #53331

ord-46fa65e8e380434ab77bc22111932839

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe reaction mixture was stirred at RT for 16 hours
  2. 2
    أخرىThe reaction mixture was quenched with H2O
  3. 3
    workup.STIRRINGstirred
  4. 4
    ترشيحThe resulting precipitate was filtered off
  5. 5
    workup.STIRRINGthe residue was stirred
  6. 6
    درجة الحرارةin refluxing methanol
  7. 7
    درجة الحرارةcooled
  8. 8
    ترشيحfiltered

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06858609B2uspto-grants-2005_02