Reaktion #357624

ord-4b8cec86b6ec498ca02f875dee378575

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe solvent was removed
  2. 2
    workup.DISSOLUTIONthe residue dissolved in ether/2M HCl
  3. 3
    SonstigeThe phases were separated
  4. 4
    workup.ADDITIONafter addition of NaOH (pH 1) to the aqueous phase, it
  5. 5
    Extraktionwas extracted with ether
  6. 6
    TrocknenThe ether phase was dried over Na2SO4
  7. 7
    Einengenconcentrated
  8. 8
    workup.DISTILLATIONDistillation by Kugelrohr

Vorschrift

To 1.17 ml (12 mmol) ethylaminoethanol in 8 ml THF were added 29.8 mg (0.3 mmol) CuCl, followed by 1 g (6.02 mmol) 1-ethynylcyclohexyl acetate. The solution was stirred at RT for 3 h, the solvent was removed and the residue dissolved in ether/2M HCl. The phases were separated, and after addition of NaOH (pH 1) to the aqueous phase, it was extracted with ether. The ether phase was dried over Na2SO4 and concentrated. Distillation by Kugelrohr yielded 2-[Ethyl-(1-ethynyl-cyclohexyl)-amino]-ethanol as colorless oil, MS: 196 (MH+).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07449483B2uspto-grants-2008_11