Reaktion #9028

ord-214ef05a35294d9a86a8c36032007d91

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction was concentrated
  2. 2
    Sonstigepurified by column chromatography on silica gel (CH2Cl2/MeOH, 9:1)

Vorschrift

To a solution of piperazine (1.444 g, 16.8 mmol) in MeOH (10 mL) was added trifluroacetic acid ethyl ester (2.0 mL, 16.8 mmol) and the mixture stirred at room temperature overnight. The reaction was concentrated and purified by column chromatography on silica gel (CH2Cl2/MeOH, 9:1) to afford the desired mono-protected piperazine adduct (1.77 g, 58%) as a pale yellow oil. 1H NMR (CDCl3) δ 1.70 (br s, 1H), 2.90–2.94 (m, 4H), 3.56–3.59 (m, 2H), 3.64–3.67 (m, 2H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091217B2uspto-grants-2006_08