Reacción #6011

ord-1d3413e2368040c69f7c5420a1d9dcb4

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaAfter cooling
  2. 2
    workup.STIRRINGthe mixture is homogenized
  3. 3
    TemperaturaIt is heated to 70°-80° C. on an oil bath
  4. 4
    workup.STIRRINGwith stirring
  5. 5
    Temperaturaheating
  6. 6
    Temperaturais maintained at a temperature of 80°-90° C. for a time T of approximately 4 h 30 min
  7. 7
    Otroon crushed ice
  8. 8
    Otrodried
  9. 9
    Lavadowashed with boiling cyclohexane
  10. 10
    Otrorecrystallized in toluene

Procedimiento

12 grams (0.09 mol) of aluminum chloride are introduced into a ground-necked flask. 3.1 cm3 (0.04 mol) of dimethylformamide are added dropwise with stirring. After cooling, two grams (0.01 mol) of benzoselenazolinone are added and the mixture is homogenized. It is heated to 70°-80° C. on an oil bath with stirring, and 0.01 to 0.012 mol of acetyl chloride is then added. heating is maintained at a temperature of 80°-90° C. for a time T of approximately 4 h 30 min. The mixture is hydrolyzed on crushed ice. The product is drained, dried, and washed with boiling cyclohexane and recrystallized in toluene.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05246951uspto-grants-1993_09