Sodium sulfate decahydrate → (1H-Indazol-3-yl)-N,N-dimethylmethanamine

HRID 2378710Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2378710
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][N:8]([CH3:20])[C:9]([C:11]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[NH:13][N:12]=1)=O.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH3:20][N:8]([CH2:9][C:11]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[NH:13][N:12]=1)[CH3:7]

Komponenten

5

Edukt 3

HCID 62649Sodium sulfate decahydrateHCID 20816326N,N-Dimethyl-1H-indazole-3-carboxamideHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 178483331(1H-Indazol-3-yl)-N,N-dimethylmethanamineAusbeute 76,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

Lithium aluminum hydride (13.7 g, 36.1 mmol) was suspended in THF (500 mL), and the suspension was added with a solution of N,N-dimethyl-1H-indazole-3-carboxamide obtained in Step 1 (34.2 g, 181 mmol) in THF (250 mL), followed by stirring at room temperature under the flow of nitrogen gas for 30 minutes. The reaction mixture was mixed with sodium sulfate decahydrate, was stirred for further 1 hour and was filtered through Celite. The solvent was evaporated under reduced pressure to obtain 3-dimethylaminomethyl-1H-indazole (24.2 g, 76%).

Aufarbeitung

  1. stirringwas stirred for further 1 hour
  2. filtrationwas filtered through Celite
  3. customThe solvent was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-88d46f27265349149ee1bd6aa3e214e1
Quelldatensatz
uspto-grants-2008_12
Patentnummer
US07470717B2

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