Reaktion #55412

ord-793b1a78e0fc48e9953bc342bff6b68e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONA suspension of 56 g
  2. 2
    TemperaturThe mixture was refluxed gently for two hours
  3. 3
    Temperaturcooled
  4. 4
    workup.STIRRINGwas stirred at 25° for 12 hours
  5. 5
    SonstigeThe mixture was evaporated
  6. 6
    Sonstigeto remove the ethanol
  7. 7
    Filtrationthe solid residue was collected by filtration

Vorschrift

A suspension of 56 g. (1.0 mol.) of potassium hydroxide and 100 g. (0.5 mol.) of 11-aminoundecanoic acid in 170 ml. of water was stirred for 30 minutes at 25° then 40 g. (0.52 mol.) of carbon disulfide and 80 ml. of ethanol were added and the reaction mixture was stirred at 25° for 12 hours. The mixture was refluxed gently for two hours and cooled. Methyl iodide (71 g., 0.3 mol.) and 130 ml. of ethanol were added to the mixture and it was stirred at 25° for 12 hours. The mixture was evaporated to remove the ethanol and the solid residue was collected by filtration to give methyl 10-carboxydecyldithiocarbamate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04220644uspto-grants-1980_09