4-Morpholinebutanenitrile → 4-(Morpholin-4-yl)butan-1-amine

HRID 56168

Reaktionsgleichung

Reaktionsgleichung von HRID 56168
[H-].[H-].[H-].[H-].[Li+].[Al+3].[O:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][C:16]#[N:17])[CH2:9][CH2:8]1>C1COCC1.O>[O:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][NH2:17])[CH2:9][CH2:8]1

Komponenten

5

Edukt 2

HCID 2945744-MorpholinebutanenitrileHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 2336114-(Morpholin-4-yl)butan-1-amine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To anhydrous THF (70 mL) was added LiAlH4 (5.37 g, 142 mmol) in one portion. The mixture was stirred at 0° C. for 20 min, and a solution of 4-morpholinobutanenitrile (7.26 g, 47 mmol) in anhydrous THF (40 mL) was added dropwise. Upon the end of addition the mixture was refluxed for 4 h, then cooled to 0° C., diluted with water (20 mL) and filtered. The filtrate was concentrated in vacuo to give the crude product for the next step without further purification.

Aufarbeitung

  1. additionUpon the end of addition the mixture
  2. temperaturewas refluxed for 4 h
  3. temperaturecooled to 0° C.
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-2c9a79470dd24e1c8cfc412f9d1e7bf0
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09434695B2

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