Reaktion #617165

ord-cf80008316be462a946c8c8f4ead7804

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturto reflux for 30 minutes
  3. 3
    Temperaturto cool
  4. 4
    TemperaturThe mixture was heated
  5. 5
    Temperaturto reflux for 4 hours
  6. 6
    SonstigeThe solvent was removed

Vorschrift

A mixture of thiourea (4.95 g, 65.0 mmol) and dimethoxymethyl-dimethyl-amine (23.2 g, 195 mmol) in methanol (80 mL) was heated to reflux for 30 minutes. After allowing the mixture to cool, triethylamine (19.8 g, 195 mmol) and a solution of 2-bromo-1-(chloro-phenyl)-ethanone (crude from last step) in methanol (50 mL) were added. The mixture was heated to reflux for 4 hours. The solvent was removed and the residue was used directly in the next procedure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09351962B2uspto-grants-2016_05