Sodium Hydroxide → 2-[4-(2-aminoethyl)piperazin-1-yl]ethanol

HRID 1064818Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1064818
[C:1]([CH2:3][N:4]1[CH2:9][CH2:8][N:7]([CH2:10][CH2:11][OH:12])[CH2:6][CH2:5]1)#[N:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>C1COCC1.C(O)C>[NH2:2][CH2:1][CH2:3][N:4]1[CH2:9][CH2:8][N:7]([CH2:10][CH2:11][OH:12])[CH2:6][CH2:5]1

Komponenten

6

Versuchsvorschrift

A solution of 4-(cyanomethyl)piperazine-1-ethanol (1.69 g, 10 mmol) in THF (20 ml) was added to a solution of lithium aluminum hydride in THF (20 ml, 20 mmol) in an argon stream with ice cooling, the mixture was stirred at room temperature for 5 minutes and heated to reflux for 90 minutes. The reaction solution was allowed to cool, diluted with ethanol with ice cooling and stirred at room temperature for 15 minutes after adding an aqueous 1N sodium hydroxide solution thereto. This was filtered off through celite and the filtrate was concentrated in vacuo to provide 4-(aminoethyl)piperazine-1-ethanol.

Aufarbeitung

  1. temperatureheated
  2. temperatureto reflux for 90 minutes
  3. temperatureto cool
  4. stirringstirred at room temperature for 15 minutes
  5. filtrationThis was filtered off through celite
  6. concentrationthe filtrate was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-539c88751648429f939d960524738f57
Quelldatensatz
uspto-grants-2005_11
Patentnummer
US06969711B2

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