Reaktion #314549

ord-018c687564df4805b3824e3c920a7679

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThis solution was warmed
  2. 2
    Temperaturto reflux
  3. 3
    Einengenconcentrated under reduced pressure
  4. 4
    SonstigeThe residue was azeotroped three times with 10 mL of benzene
  5. 5
    Sonstigeto remove any remaining thionyl chloride
  6. 6
    Sonstigeused without further purification

Vorschrift

To a flask containing 2,2,3,3-tetramethylcyclopropane carboxylic acid (Aldrich, 13.5 g, 95 mmol) was added 30 mL of thionyl chloride (410 mmol, excess). This solution was warmed to reflux and stirred for 2 h. The mixture was then cooled to ambient temperature and concentrated under reduced pressure. The residue was azeotroped three times with 10 mL of benzene to remove any remaining thionyl chloride, and used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07560481B2uspto-grants-2009_07