Reaktion #1519695

ord-c0101af3432a49f284274d69e85e6902

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe reaction mixture was heated at 60° for 48 hours
  2. 2
    SonstigeThe solvent was evaporated under reduced pressure
  3. 3
    WaschenWashed with water
  4. 4
    ExtraktionExtracted into 2M hydrochloric acid
  5. 5
    Waschenwashed with dichloromethane
  6. 6
    workup.ADDITIONBasified to pH 10 by addition of 2M sodium hydroxide
  7. 7
    ExtraktionExtracted with diethyl ether
  8. 8
    Waschenwashed with water
  9. 9
    TrocknenDried over anhydrous magnesium sulphate
  10. 10
    Sonstigeevaporated the solvent under reduced pressure

Vorschrift

(+)-Limonene oxide (13.2 g, 0.087 moles) was dissolved in ethanol (40 ml) and lithium chloride (5.9 g, 0.14 moles) was added with stirring. Morpholine (11.4 g, 0.13 moles) was added and the reaction mixture was heated at 60° for 48 hours. The solvent was evaporated under reduced pressure and the residue taken up in dichloromethane. Washed with water. Extracted into 2M hydrochloric acid and washed with dichloromethane. Basified to pH 10 by addition of 2M sodium hydroxide. Extracted with diethyl ether and washed with water. Dried over anhydrous magnesium sulphate and evaporated the solvent under reduced pressure to give the product as a yellow oil (10.3 g)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07612101B2uspto-grants-2009_11