Potassium Cyanide → HCID 86671305, Verbindung

HRID 2367890

Reaktionsgleichung

Reaktionsgleichung von HRID 2367890
[CH3:1][N:2]([CH3:11])[N:3]1[CH2:8][CH2:7][C:6](=[N:9][OH:10])[CH2:5][CH2:4]1.P([O-])(O)(O)=O.[K+].[C-:18]#[N:19].[K+]>O>[CH3:1][N:2]([CH3:11])[N:3]1[CH2:8][CH2:7][C:6]([NH:9][OH:10])([C:18]#[N:19])[CH2:5][CH2:4]1

Komponenten

5

Edukt 3

HCID 9032Potassium CyanideHCID 516951Monobasic potassium phosphateHCID 866713041-Dimethylamino-piperidin-4-one oxime

Produkt 1

HCID 86671305HCID 86671305, VerbindungAusbeute 53,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

12.4 g 1-Dimethylamino-piperidin-4-one oxime (from Step 1) is dissolved in 160 ml water. 49.3 g potassium dihydrogenphosphate is added. The resulting yellow suspension is cooled to 5° C., and a solution of 11.24 g potassium cyanide in 40 ml water is added. The mixture is stirred at room temperature for 2 days, then extracted with ethyl acetate, the organic layer dried over sodium sulfate, and the solvent evaporated, to give 7.8 g 1-Dimethylamino-4-hydroxyamino-piperidine-4-carbonitrile. 1H-NMR (CDCl3): 5.60 ppm (s, broad, 1H), 5.10 ppm (s, broad, 1H), 2.92 ppm (m, 2H), 2.61 ppm (m, 2H), 2.33 ppm (s, 6H), 2.10 ppm (m, 2H), 1.70 ppm (m, 2H).

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. dry with materialthe organic layer dried over sodium sulfate
  3. customthe solvent evaporated

Quellen und Nachweise

ORD-Eintrag
ord-16d1c233e8934ee3b70bd591f0308c4d
Quelldatensatz
uspto-grants-2014_04
Patentnummer
US08703165B2

Verknüpfte Notizen

Wird geladen…