Reaktion #69575

ord-bf2fd9e410f04d93a4349fdd3db647df

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe mixture was concentrated to dryness
  2. 2
    Sonstigethe residue triturated with diethyl ether
  3. 3
    Filtrationthe solid collected by filtration

Vorschrift

To a solution of 1,1-dimethylethyl (3R)-3-methyl-4-{[4-(trifluoromethyl)phenyl]sulfonyl}-1-piperazinecarboxylate (may be prepared as described in Description 6) (3.39 g, 8.30 mmol) in 1,4-dioxane (20 ml) was added HCl (4M in 1,4-dioxane) (10.37 ml, 41.5 mmol) and the resultant mixture stirred under an atmosphere of Ar for 16 hours. A further 5 ml of 4M HCl in dioxane was added and the mixture stirred at room temperature for 72 hours. The mixture was concentrated to dryness and the residue triturated with diethyl ether and the solid collected by filtration giving the title compound (2.507 g) as a white powder.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08530478B2uspto-grants-2013_09