Reaktion #51634

ord-14089d6065474121a1b9c499e0722165

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture is heated
  2. 2
    Temperaturunder reflux until completion of the reaction (5-12 hours)
  3. 3
    Filtrationis filtered off
  4. 4
    Waschenwashed with water
  5. 5
    SonstigeThe crude material is purified by usual silica gel chromatography

Vorschrift

A solution of bromo(4-nitrophenyl)acetaldehyde and potassium thiocyanate (1.2 equivalents) in methanol is stirred at room temperature for 1 hour. The cyclohexylamine (1,05 equivalents) is added drop-wise and the mixture is heated under reflux until completion of the reaction (5-12 hours). After cooling to 0° C. the precipitate is filtered off and washed with water. The crude material is purified by usual silica gel chromatography to give the desired compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06852720B2uspto-grants-2005_02