Sodium sulfate decahydrate → 2-(4-Benzylpiperazin-1-yl)ethan-1-amine

HRID 1162342Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1162342
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[CH2:19][CH2:18][N:17]([CH2:20][C:21]#[N:22])[CH2:16][CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH2:7]([N:14]1[CH2:15][CH2:16][N:17]([CH2:20][CH2:21][NH2:22])[CH2:18][CH2:19]1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

Komponenten

5

Edukt 3

HCID 62649Sodium sulfate decahydrateHCID 38557212-(4-Benzylpiperazin-1-yl)acetonitrileHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 27353312-(4-Benzylpiperazin-1-yl)ethan-1-amineAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel3×

Versuchsvorschrift

To a suspension of lithium aluminum hydride (5.0 g) in anhydrous THF (150 ml) was added a solution of (4-benzyl-1-piperazinyl)acetonitrile (11 g) obtained in Example 95a) in anhydrous THF (50 ml) under ice-cooling. The reaction solution was refluxed for 3 hours, to the reaction solution was then added sodium sulfate decahydrate (420 g) under ice-cooling, and mixed for 15 hours. The reaction solution was diluted with THF, the precipitate obtained by decantation was filtered off, and the solvent was distilled off under reduced pressure to obtain the title compound as pale yellow liquid (10 g, 95%).

Aufarbeitung

  1. temperaturecooling
  2. temperatureThe reaction solution was refluxed for 3 hours, to the reaction solution
  3. additionmixed for 15 hours
  4. customthe precipitate obtained by decantation
  5. filtrationwas filtered off
  6. distillationthe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-b8dd6ce48ac149cba9524242005e5ca5
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07820673B2

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