반응 #53331

반응 방정식

NaOH

guanidine

intermediate ( 27 )

4-[[4-chloro-6-[(2,6-dichlorophenyl)methyl]-1,3,5-triazin-2-yl]-amino]benzonitrile

→

N-[4-[(4-cyanophenyl)amino]-6-[(2,6-dichlorophenyl)methyl]-1,3,5-triazin-2-yl]-guanidine

수율 64.3%

용매

1,4-dioxane

반응 조건

후처리

1. 1
   workup.STIRRINGthe reaction mixture was stirred at RT for 16 hours
2. 2
   기타The reaction mixture was quenched with H2O
3. 3
   workup.STIRRINGstirred
4. 4
   여과The resulting precipitate was filtered off
5. 5
   workup.STIRRINGthe residue was stirred
6. 6
   온도in refluxing methanol
7. 7
   온도cooled
8. 8
   여과filtered

실험 절차

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).

출처