반응 #533101

반응 방정식

5-chloro-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-6-amine

(4-aminophenyl)(morpholino)methanone

N,N-diisopropylethylamine

→

(4-(6-amino-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-5-ylamino)phenyl)(morpholino)methanone

수율 33.9%

용매

1,4-dioxane

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux for 2 days
3. 3
   기타The volatiles were removed under vacuum
4. 4
   workup.ADDITIONTo the residue was added water (60 mL)
5. 5
   여과The precipitating material was collected by suction filtration
6. 6
   기타The filter cake was purified by ISCO (120 g silica gel, solid loading, 3-8% MeOH/CH2Cl2)

실험 절차

A mixture of 5-chloro-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-6-amine (1.05 g, 3.95 mmol), (4-aminophenyl)(morpholino)methanone (1.630 g, 7.90 mmol), and N,N-diisopropylethylamine (1.243 mL, 7.11 mmol) in 1,4-dioxane (60 mL) was heated at reflux for 2 days. The volatiles were removed under vacuum. To the residue was added water (60 mL). The precipitating material was collected by suction filtration. The filter cake was purified by ISCO (120 g silica gel, solid loading, 3-8% MeOH/CH2Cl2) to provide the desired product, (4-(6-amino-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-5-ylamino)phenyl)(morpholino)methanone (0.595 g, 1.339 mmol, 33.9% yield), as a yellow solid.

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