Реакция #6011

ord-1d3413e2368040c69f7c5420a1d9dcb4

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураAfter cooling
  2. 2
    workup.STIRRINGthe mixture is homogenized
  3. 3
    ТемператураIt is heated to 70°-80° C. on an oil bath
  4. 4
    workup.STIRRINGwith stirring
  5. 5
    Температураheating
  6. 6
    Температураis maintained at a temperature of 80°-90° C. for a time T of approximately 4 h 30 min
  7. 7
    Другоеon crushed ice
  8. 8
    Другоеdried
  9. 9
    Промывкаwashed with boiling cyclohexane
  10. 10
    Другоеrecrystallized in toluene

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05246951uspto-grants-1993_09