Reaktion #45057

ord-7cd9b3c6ffb040d58b94fc1a4073fa4f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction mixture was filtered
  2. 2
    Waschenwashed with ether
  3. 3
    Sonstigeto afford crude 1-cyclopropylpiperazine (0.659 g) as a white solid
  4. 4
    SonstigeThe crude product was purified by ion exchange chromatography
  5. 5
    WaschenThe desired product was eluted from the column
  6. 6
    Sonstigewere evaporated to dryness

Vorschrift

A solution of tert-butyl 4-cyclopropylpiperazine-1-carboxylate (0.792 g, 3.50 mmol) in 4M HCl in 1,4-dioxane (4.37 mL, 17.50 mmol) was stirred at room temperature for 3 h under nitrogen. The reaction mixture was filtered and washed with ether to afford crude 1-cyclopropylpiperazine (0.659 g) as a white solid. The crude product was purified by ion exchange chromatography, using a SCX column. The desired product was eluted from the column using 3.5M NH3/MeOH and pure fractions were evaporated to dryness to afford 1-cyclopropylpiperazine (0.264 g, 59.7%) as a yellow oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737149B2uspto-grants-2010_06