반응 #64673

ord-9f9292b5befb4595a3e0f33675685eb0

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the resulting mixture heated
  2. 2
    온도under reflux for 16 hours
  3. 3
    온도The mixture was then cooled
  4. 4
    기타quenched on to water (250 ml)
  5. 5
    여과The solid was filtered
  6. 6
    세척washed with water the resulting damp solid
  7. 7
    기타recrystallised from ethanol (50 ml)

실험 절차

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%

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05414092uspto-grants-1995_05