Reaktion #684208

ord-52c173ef593d468097ab647fd57f1bfc

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled in a dry-ice-acetone bath
  2. 2
    Sonstigethe excess ammonia is evaporated
  3. 3
    workup.DISSOLUTIONthe reaction mixture is dissolved in water
  4. 4
    Extraktionextracted with ether which
  5. 5
    Waschenis washed with water
  6. 6
    Trocknendried over magnesium sulfate
  7. 7
    Sonstigeevaporated at reduced pressure

Vorschrift

To a stirred suspension of 2-cyclopentyl-2-methyl-5-methylthio-6,7-dichloro-1-indanone (3.59 g., 0.01 mole) in liquid ammonia (100 ml.) cooled in a dry-ice-acetone bath is added sodium (460 mg., 0.02 gr. atom) in small portions until a permanent blue color persists. Ammonium chloride (1.0 g.) is added, the excess ammonia is evaporated and the reaction mixture is dissolved in water, acidified and extracted with ether which is washed with water, dried over magnesium sulfate and evaporated at reduced pressure affording 2-cyclopentyl-2-methyl-5-mercapto-6,7-dichloro-1-indanone.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04012524uspto-grants-1977_03