Reaktion #546923

ord-b41610da23d04c1baa346187642f635e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe product is extracted with dichloromethane
  2. 2
    TrocknenThe organic phase is dried over sodium sulphate
  3. 3
    Filtrationby filtering
  4. 4
    Einengenconcentrating under vacuum
  5. 5
    Sonstigethe residue is purified on a silica column (eluent: CH2Cl2/EtOH: 4/1)
  6. 6
    SonstigeA clear oil is obtained with a yield of 84% (0.84 g)

Vorschrift

4-(N-methylpiperazinyl)aniline (0.5 g; 2.6 mmol), hydroxybenzotriazole (0.39 g; 2.86 mmol), 1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide hydrochloride (1.1 g; 5.7 mmol) and triethylamine (0.8 ml; 5.7 mmol) are added to a solution of 0.55 g (2.6 mmol) of 4-(4-nitrophenyl)butanoic acid in dichloromethane (30 ml). The reaction medium is stirred for 16 hours at ambient temperature, then the medium is diluted with 15 ml of water and the product is extracted with dichloromethane. The organic phase is dried over sodium sulphate followed by filtering and concentrating under vacuum and the residue is purified on a silica column (eluent: CH2Cl2/EtOH: 4/1). A clear oil is obtained with a yield of 84% (0.84 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07196084B2uspto-grants-2007_03