반응 #1110711

반응 방정식

Hydrazine hydrate

2-[(2,5-dimethylphenyl)oxy]-5-nitropyridine

Intermediate 33

2-[(2,5-dimethylphenyl)oxy]-5-nitropyridine

→

title compound

수율 88.2%

6-[(2,5-dimethylphenyl)oxy]-3-pyridinamine

수율 88.2%

용매

ethanol

반응 조건

후처리

1. 1
   온도The reaction mixture was heated
2. 2
   온도at reflux under argon
3. 3
   온도After overnight heating
4. 4
   온도the reaction was cooled down
5. 5
   여과The reaction mixture was filtered
6. 6
   기타The organic phase was evaporated under vacuum
7. 7
   기타The residue was purified by SCX (wash with MeOH, desorbed with 2N methanolic ammonia)
8. 8
   기타Evaporation

실험 절차

2-[(2,5-dimethylphenyl)oxy]-5-nitropyridine (Intermediate 33, 140 mg, 0.450 mmol) was dissolved in ethanol (3 mL). Hydrazine hydrate (83 μL, 0.884 mmol) and palladium on carbon (47 mg, 0.044 mmol) were added. The reaction mixture was heated at reflux under argon. After overnight heating, the reaction was cooled down. The reaction mixture was filtered. The organic phase was evaporated under vacuum. The residue was purified by SCX (wash with MeOH, desorbed with 2N methanolic ammonia). Evaporation afforded the title compound (85 mg).

출처