Reaktion #365728

ord-e8e5126dd3414b259b97b87086a30370

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with dichloromethane
  2. 2
    WaschenThe extract was washed with water
  3. 3
    Sonstigedried
  4. 4
    Einengenconcentrated
  5. 5
    SonstigeThe residue was crystallized from diisopropylether

Vorschrift

To a mixture of aqueous sodium hydrogen carbonate (10 ml) solution, 1-tert-butoxycarbonylpiperazine (1.0 g) and ethyl acetate (10 ml), was added 6-chloronaphthalene-2-sulfonylchloride (1.4 g) and the mixture was stirred at room temperature for 1 hour and extracted with dichloromethane. The extract was washed with water, dried and concentrated. The residue was crystallized from diisopropylether to give colorless crystals of 1-(tert-butoxycarbonyl)-4-(6-chloro-naphthalene-2-sulfonyl)piperazine (2.02 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06359134B1uspto-grants-2002_03