تفاعل #6011

ord-1d3413e2368040c69f7c5420a1d9dcb4

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling
  2. 2
    workup.STIRRINGthe mixture is homogenized
  3. 3
    درجة الحرارةIt is heated to 70°-80° C. on an oil bath
  4. 4
    workup.STIRRINGwith stirring
  5. 5
    درجة الحرارةheating
  6. 6
    درجة الحرارةis maintained at a temperature of 80°-90° C. for a time T of approximately 4 h 30 min
  7. 7
    أخرىon crushed ice
  8. 8
    أخرىdried
  9. 9
    غسيلwashed with boiling cyclohexane
  10. 10
    أخرىrecrystallized in toluene

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05246951uspto-grants-1993_09