تفاعل #53328

معادلة التفاعل

Intermediate ( 27 )

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

O-(trimethylsilyl)hydroxyl-amine

→

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

المردود 59.8%

المذيبات

1,4-dioxane

ظروف التفاعل

المعالجة

1. 1
   تركيزThe reaction mixture was concentrated
2. 2
   workup.ADDITIONDCM (50 ml), NaOH (1 N; 50 ml), and HCl (1N; 100 ml) were added
3. 3
   workup.STIRRINGThe solution was stirred for one hour
4. 4
   ترشيحThe precipitate was filtered off
5. 5
   أخرىrecrystallized from methanol
6. 6
   ترشيحThe precipitate was filtered off
7. 7
   أخرىdried

الإجراء التجريبي

Intermediate (27) (0.0128 mol), 1,4-dioxane (50 ml), and O-(trimethylsilyl)hydroxyl-amine, (0.134 mol) were combined under argon. The reaction mixture was stirred at RT for 20 hours. The reaction mixture was concentrated and DCM (50 ml), NaOH (1 N; 50 ml), and HCl (1N; 100 ml) were added. The solution was stirred for one hour. The precipitate was filtered off and recrystallized from methanol. The precipitate was filtered off and dried, yielding 2.96 g (59.8%) of 4-[[4-[(2,6-dichlorophenyl)methyl]-6-(hydroxyamino)-1,3,5-triazin-2-yl] amino]benzonitrile monohydrochloride.monohydrate (compound 21).

المصدر