Reaktion #544754

ord-404738228c6c445aa5fa02486a4e59c2

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationthe solids were collected by filtration
  2. 2
    workup.DISSOLUTIONdissolved in aqueous 1 N NaOH (300 mL)
  3. 3
    ExtraktionThe aqueous solution was extracted with ethyl acetate (3×50 mL)
  4. 4
    WaschenThe combined organic layers were washed with brine
  5. 5
    Trocknendried over anhydrous magnesium sulfate
  6. 6
    Filtrationfiltered
  7. 7
    Sonstigeevaporated

Vorschrift

To a stirred solution of 1-(2-chloro-4-nitrophenyl)-4-methylpiperazine (2.43 g, 9.5 mmol) in 2N HCl (35 mL) at RT was added tin (II) chloride (7.2 g, 38 mmol). After 1 h, the solids were collected by filtration and dissolved in aqueous 1 N NaOH (300 mL). The aqueous solution was extracted with ethyl acetate (3×50 mL). The combined organic layers were washed with brine, dried over anhydrous magnesium sulfate, filtered, and evaporated to afford the title compound (2.02 g, 95%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07189712B2uspto-grants-2007_03