Reaktion #64673

ord-9f9292b5befb4595a3e0f33675685eb0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe resulting mixture heated
  2. 2
    Temperaturunder reflux for 16 hours
  3. 3
    TemperaturThe mixture was then cooled
  4. 4
    Sonstigequenched on to water (250 ml)
  5. 5
    FiltrationThe solid was filtered
  6. 6
    Waschenwashed with water the resulting damp solid
  7. 7
    Sonstigerecrystallised from ethanol (50 ml)

Vorschrift

1-Chloro-4-hydroxythioxanthone (7.8 g; 0.03 mol) prepared as above and potassium carbonate (5.0 g; 0.036 mol) was stirred and refluxed for 10 minutes in acetone (50 ml). n-Propyl bromide (5.5 g; 0.045 mol) was added and the resulting mixture heated under reflux for 16 hours. The mixture was then cooled and quenched on to water (250 ml). The solid was filtered and washed with water the resulting damp solid recrystallised from ethanol (50 ml) to afford the title compound (6.9 g; 75.5%) of mp 102°-3°. Analysis C16H13ClO2S=304.777 Requires C 63.05%; H 4.30%; Cl 11.63%; S 10.52% Found C 63.14%; H 4.37%; Cl 11.66%; S 10.63%

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05414092uspto-grants-1995_05