Reaktion #63429

ord-2e83975f0e96488ea92c443cccb3aac6

Reaktionsgleichung

Reagenzien

Keine

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONthe layers were mixed
  2. 2
    Einengento saturate the aqueous layer
  3. 3
    SonstigeThe organic layer was collected
  4. 4
    Extraktionthe aqueous layer was extracted three more times with petroleum ether
  5. 5
    SonstigeThe combined organic layers were transferred to a 500 ml round bottom flask
  6. 6
    workup.ADDITIONwere added
  7. 7
    Sonstigethe petroleum ether was removed by distillation

Vorschrift

Ten grams of arecoline HBr was dissolved in a minimal quantity (approximately 25 ml) of water and adjusted to pH 10 with saturated KOH in a separatory funnel. One hundred mls of petroleum ether was added and the layers were mixed. NaCl was then added to saturate the aqueous layer. The organic layer was collected, and the aqueous layer was extracted three more times with petroleum ether. The combined organic layers were transferred to a 500 ml round bottom flask, boiling chips were added and the petroleum ether was removed by distillation. The remaining oil was layered with N2 and stored in low-actinic glassware. The oil was anlyzed by NMR to show the absence of a halogen component.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04765985uspto-grants-1988_08