Reaktion #6011

ord-1d3413e2368040c69f7c5420a1d9dcb4

Reaktionsgleichung

CC(=O)Cl
acetyl chloride
[Al+3].[Cl-].[Cl-].[Cl-]
aluminum chloride
CN(C)C=O
dimethylformamide
O=[Se]1C=Nc2ccccc21
benzoselenazolinone
CC(=O)c1ccc2c(c1)[Se](=O)C=N2
6-Acetylbenzoselenazolinone

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    workup.STIRRINGthe mixture is homogenized
  3. 3
    TemperaturIt is heated to 70°-80° C. on an oil bath
  4. 4
    workup.STIRRINGwith stirring
  5. 5
    Temperaturheating
  6. 6
    Temperaturis maintained at a temperature of 80°-90° C. for a time T of approximately 4 h 30 min
  7. 7
    Sonstigeon crushed ice
  8. 8
    Sonstigedried
  9. 9
    Waschenwashed with boiling cyclohexane
  10. 10
    Sonstigerecrystallized in toluene

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05246951uspto-grants-1993_09