Reacción #314393

ord-80a9f63cf4254dba87ce869e167cfda3

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otro1-Chloro-4-dodecyloxythioxanthone was prepared
  2. 2
    Temperaturarefluxed for 10 min
  3. 3
    Temperaturaunder reflux
  4. 4
    Otroquenched with water (500 mL)
  5. 5
    FiltraciónThe obtained solid was filtered
  6. 6
    Lavadowashed with water
  7. 7
    Otropurified
  8. 8
    Otroby recrystallized from isopropanol

Procedimiento

1-Chloro-4-dodecyloxythioxanthone was prepared as follows. A solution of 1-chloro-4-hydroxythioxanthone (14.0 g, 0.05 mol), K2CO3 (8.0 g, 0.06 mol) in acetone (250 mL) was stirred and refluxed for 10 min. Bromododecane (20.0 g, 0.08 mol) was added and the resulting mixture was stirred for 24 h under reflux. The reaction was then cooled to room temperature and quenched with water (500 mL). The obtained solid was filtered, washed with water, purified by recrystallized from isopropanol to give the 1-chloro-4-dodecyloxythioxanthone (14.3 g, 62%) with mp 79-80° C. The identity of this compound was shown by 1H NMR to have the following structure:

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07560219B2uspto-grants-2009_07