Reaktionsgleichung
[CH:1]1([C:4]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][C:11]=3[N+:13]([O-])=O)[N:6]([CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([CH3:23])[N:18]=3)[N:5]=2)[CH2:3][CH2:2]1>[Pd].C1(C)C=CC=CC=1>[CH:1]1([C:4]2[C:12]3[C:11]([NH2:13])=[CH:10][CH:9]=[CH:8][C:7]=3[N:6]([CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([CH3:23])[N:18]=3)[N:5]=2)[CH2:2][CH2:3]1Komponenten
4
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 75 °C
Versuchsvorschrift
3-Cyclopropyl-1-((6-methylpyridin-2-yl)methyl)-4-nitro-1H-indazole (17.0 g, 55.1 mmol) and 10% Pd/C (1.2 g, 0.6 mmol) were added to toluene (170 mL) in an autoclave. The solution was stirred under 40 psi of H2 at 75° C. for 18 hours. The catalyst was removed by filtration through Celite® and the filter cake was rinsed with toluene (34 mL). The filtrate was concentrated to about 35 mL and heptane (85 mL) was added to the filtrate to precipitate the product which was collected by vacuum filtration and dried under vacuum for 18 hours to afford 3-cyclopropyl-1-((6-methylpyridin-2-yl)methyl)-1H-indazol-4-amine (12.2 g).
Aufarbeitung
- customThe catalyst was removed by filtration through Celite®
- washthe filter cake was rinsed with toluene (34 mL)
- concentrationThe filtrate was concentrated to about 35 mL and heptane (85 mL)
- additionwas added to the filtrate
- customto precipitate the product which
- filtrationwas collected by vacuum filtration
- customdried under vacuum for 18 hours
Quellen und Nachweise
- ORD-Eintrag
- ord-8b1baa9a4c414152956b97c6f6e31739
- Quelldatensatz
- uspto-grants-2014_09
- Patentnummer
- US08841455B2
Verknüpfte Notizen
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