Reaktion #991315

ord-3e15dd91e10f4725a615ec51c314e2ef

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with 200 ml water
  2. 2
    Trocknendried (MgSO4)
  3. 3
    SonstigeThe solvent was evaporated
  4. 4
    Sonstigea brown oil was recovered
  5. 5
    Sonstigerecrystallized in ethanol

Vorschrift

To a 200-ml methylene solution of 4,4-dimethylhomophthalimide (33.5 g) and 1,1,2,2-tetrachloroethyl sulfenyl chloride (42.2 g) at 0° C. was added dropwise 18.2 g triethylamine over 5 minutes. The mixture was stirred for 4 hours, washed with 200 ml water and dried (MgSO4). The solvent was evaporated and a brown oil was recovered, recrystallized in ethanol to yield 54 g (78%) tan solid, m.p. 112°-113° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04230711uspto-grants-1980_10