Water → N-Benzylputrescine

HRID 1493887Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1493887
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([CH2:9][CH2:10][CH2:11][NH:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)#[N:8].O.[OH-].[Na+]>O1CCCC1>[CH2:13]([NH:12][CH2:11][CH2:10][CH2:9][CH2:7][NH2:8])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 30145704-(Benzylamino)butanenitrileHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 152999N-BenzylputrescineAusbeute 57,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a suspension of 1.1 g of lithium aluminum hydride in 50 ml of tetrahydrofuran was added slowly 2.9 g of N-(3-cyanopropyl)benzylamine (obtained in Reference Example 4) at room temperature. The reaction mixture was heated gently under reflux for 15 minutes and then allowed to cool. To the mixture was added dropwise and carefully 2.2 ml of water and then 1.8 ml of 10% aqueous sodium hydroxide. The resultant precipitate was filtered off, the filtrate was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure to give 1.7 g of N-benzyl-1,4-butanediamine as a colorless oil.

Aufarbeitung

  1. temperatureThe reaction mixture was heated gently
  2. temperatureunder reflux for 15 minutes
  3. temperatureto cool
  4. additionTo the mixture was added dropwise
  5. filtrationThe resultant precipitate was filtered off
  6. dry with materialthe filtrate was dried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d583353b775646039a92d8465ca5e4ec
Quelldatensatz
uspto-grants-1991_06
Patentnummer
US05025033

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