Reaktion #1435746

ord-96af6633f0ff44f3afb9eaf504ffa333

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with diethyl ether
  2. 2
    TrocknenThe extract was dried with sodium sulfate
  3. 3
    Einengenconcentrated
  4. 4
    Sonstigeto give a pale yellow solid

Vorschrift

Dimethyl-[1-(4-nitro-phenyl)-piperidin-4-yl]-amine (Example 2, 1.1 g, 5.0 mmol) was dissolved in DMF (5 mL). To the stirred solution, thiocarbonyl diimidazole (Aldrich, 1.18 g, 90%, 6 mmol) was added and the solution was stirred at room temperature for 80 minutes. The mixture was poured into water and extracted with diethyl ether. The extract was dried with sodium sulfate and concentrated to give a pale yellow solid. 1.12 g, 85%. MS (m+H)+: 262.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07211576B2uspto-grants-2007_05