1,3-Dioxolane-2-propylamine → 3-(3-[1,3]Dioxolan-2-yl-propylamino)butyronitrile

HRID 888759

Reaktionsgleichung

Reaktionsgleichung von HRID 888759
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[CH2:6][CH2:7][CH2:8][NH2:9].[C:10](#[N:14])/[CH:11]=[CH:12]/[CH3:13]>C(OCC)(=O)C>[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[CH2:6][CH2:7][CH2:8][NH:9][CH:12]([CH3:13])[CH2:11][C:10]#[N:14]

Komponenten

4

Edukt 2

HCID 780991,3-Dioxolane-2-propylamineHCID 637921Crotononitrile

Produkt 1

HCID 688630333-(3-[1,3]Dioxolan-2-yl-propylamino)butyronitrileAusbeute 92,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

49.85 g (0.38 mol) of 3-[1,3]-dioxolan-2-yl-propylamine and 43.34 g (0.646 mol) of crotono-nitrile are combined in a 200 ml round-bottomed flask and heated at 100° C. for 72 hours. After cooling, the brown mass is diluted with ethyl acetate and washed with water. The organic phase is dried over calcium carbonate and purified by filtration on silica gel (eluent: ethyl acetate). Evaporation of the solvent gives 69.8 g of 3-(3-[1,3]-dioxolan-2-yl-propylamino)butyronitrile as a reddish liquid which is used without further purification in the next stage.

Aufarbeitung

  1. temperatureAfter cooling
  2. washwashed with water
  3. dry with materialThe organic phase is dried over calcium carbonate
  4. filtrationpurified by filtration on silica gel (eluent: ethyl acetate)
  5. customEvaporation of the solvent

Quellen und Nachweise

ORD-Eintrag
ord-b17d6a09186343188dcfe257dc075376
Quelldatensatz
uspto-grants-2012_08
Patentnummer
US08252784B2

Verknüpfte Notizen

Wird geladen…