Reaktion #332112

ord-52f5f3f1ba75403a96b8ba283fab6ef9

Lösungsmittel

Reaktionsbedingungen

Temperatur
85°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool
  2. 2
    Extraktionextracted with hexane
  3. 3
    Waschenthe extract was washed with saturated aqueous sodium chloride
  4. 4
    EinengenThe organic layer was concentrated under reduced pressure

Vorschrift

6.24 g (26.0 mmol) of 2-chloro-N-(2-methyl-1-p-tolylpropan-2-yl)acetamide and 1.98 g (26.0 mmol) of thiourea were dissolved in 50 mL of ethanol, and 10.2 mL of acetic acid was added dropwise at room temperature. After 3 hours of stirring at 85° C. the resulting white suspension was allowed to cool and diluted with 300 mL of water. The reaction solution was basified with 20 wt % aqueous sodium hydroxide and extracted with hexane, and the extract was washed with saturated aqueous sodium chloride. The organic layer was concentrated under reduced pressure to give 4.04 g of the desired product as a yellow green liquid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08658686B2uspto-grants-2014_02