反応 #63429

ord-2e83975f0e96488ea92c443cccb3aac6

試薬

なし

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04765985uspto-grants-1988_08