Nitrogen → 83962-01-0

HRID 1044736Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1044736
N#N.[CH3:3][C:4]1([CH2:9][CH2:10][CH2:11][C:12]#[N:13])[O:8][CH2:7][CH2:6][O:5]1.[H-].[H-].[H-].[H-].[Li+].[Al+3].[OH-].[Na+]>CCOCC.O>[CH3:3][C:4]1([CH2:9][CH2:10][CH2:11][CH2:12][NH2:13])[O:5][CH2:6][CH2:7][O:8]1

Komponenten

7

Edukt 4

HCID 947NitrogenHCID 14798Sodium HydroxideHCID 155808174-(2-Methyl-1,3-dioxolan-2-yl)butanenitrileHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 1558081883962-01-0

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 4-(2-methyl-[1,3]dioxolan-2-yl)-butyronitrile (2.23 g, 14.4 mmol) in dry Et2O (2.5 mL) was added to a suspension of LiAlH4 (1.36 g, 35.9 mmol) in dry Et2O (50 mL). The reaction mixture was stirred at reflux for 3 h, cooled down to rt and treated with water (2 mL), 15% aq. NaOH (2 mL) and water (4 mL). The precipitate was filtered off and washed with Et2O. The filtrate was dried over Na2SO4, filtered and concentrated under reduced pressure to give the title compound as a light brown oil. LC-MS-conditions 02: tR=0.32 min; [M+H]+=160.29.

Aufarbeitung

  1. temperatureat reflux for 3 h
  2. filtrationThe precipitate was filtered off
  3. washwashed with Et2O
  4. dry with materialThe filtrate was dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7bacf699e9294bd48091ab86dd6a6ee9
Quelldatensatz
uspto-grants-2013_10
Patentnummer
US08563714B2

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