반응 #6011

ord-1d3413e2368040c69f7c5420a1d9dcb4

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling
  2. 2
    workup.STIRRINGthe mixture is homogenized
  3. 3
    온도It is heated to 70°-80° C. on an oil bath
  4. 4
    workup.STIRRINGwith stirring
  5. 5
    온도heating
  6. 6
    온도is maintained at a temperature of 80°-90° C. for a time T of approximately 4 h 30 min
  7. 7
    기타on crushed ice
  8. 8
    기타dried
  9. 9
    세척washed with boiling cyclohexane
  10. 10
    기타recrystallized in toluene

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05246951uspto-grants-1993_09