Reaktionsgleichung
[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][C:5]1[CH:13]=[CH:12][C:11](N)=[C:10]2[C:6]=1[CH:7]=[N:8][NH:9]2.S(=O)(=O)(O)[OH:17].C(=O)(O)[O-].[Na+]>>[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][C:5]1[CH:13]=[CH:12][C:11]([OH:17])=[C:10]2[C:6]=1[CH:7]=[N:8][NH:9]2Komponenten
4
Versuchsvorschrift
In an autoclave, 1.2 g of N,N-dimethyl-N-[2-(7-amino-1H-indazol-4-yl)ethyl]amine and 24 ml of 1N sulfuric acid are heated under argon for 16 hours to 180° C. Subsequently the mixture is combined under ice cooling with sodium bicarbonate and extracted by shaking with ethyl acetate/butanol (10:1). The organic phase is dried, concentrated, and the residue is triturated with ethyl acetate, thus obtaining 700 mg of N,N-dimethyl-N-[2-(7-hydroxy-1H-indazol-4-yl)ethyl]amine, mp 233°-234° C., yielding after treatment with methanol and ethereal hydrochloric acid, and recrystallization from methanol/diethyl ether, 680 mg of N,N-dimethyl-N-[2-(7-hydroxy-1H-indazol-4-yl)ethyl]amine, hydrochloride, mp 223°-227° C.
Aufarbeitung
- extractionextracted
- customThe organic phase is dried
- concentrationconcentrated
- customthe residue is triturated with ethyl acetate
Quellen und Nachweise
- ORD-Eintrag
- ord-32cbd6824bc2499ba13a8bed93d8e428
- Quelldatensatz
- uspto-grants-1990_09
- Patentnummer
- US04958026
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