Reaktion #60453

ord-369d6936f64943aba1f9b932445c8d80

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    WaschenThe separated organic layer was washed with water and brine in that order
  2. 2
    Trocknendried over anhydrous sodium sulfate
  3. 3
    FiltrationThe desiccant was filtered off
  4. 4
    Einengenthe filtrate was concentrated under reduced pressure
  5. 5
    SonstigeThe residue was dried under reduced pressure

Vorschrift

A mixture of 4-[4-bromo-2-(4,4-dimethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester (1.5 g, 3.32 mmol) produced in Example (3e), trifluoroacetic acid (3 mL, 38.7 mmol) and dichloromethane (6 mL) was stirred for 2 hours and 30 minutes at room temperature. Saturated aqueous solution of sodium carbonate was added to the reaction mixture and extraction was performed with ethyl acetate. The separated organic layer was washed with water and brine in that order and then dried over anhydrous sodium sulfate. The desiccant was filtered off and the filtrate was concentrated under reduced pressure. The residue was dried under reduced pressure to give 1.21 g of a crude product of the title compound as a brown oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07425554B2uspto-grants-2008_09