تفاعل #1747866

ord-eee27b9e4fe147dd8e55086696d664d8

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةto reflux temperature
  3. 3
    درجة الحرارةheated
  4. 4
    ترشيحthe reaction mixture was filtered
  5. 5
    تركيزThe filtrate was concentrated
  6. 6
    درجة الحرارةcooled in an ice bath, in the course of which a solid
  7. 7
    أخرىprecipitated out
  8. 8
    أخرىThis was removed by means of a blue-band filter
  9. 9
    أخرىdried
  10. 10
    أخرىThe crude product (23.22 g) was recrystallized from 70 ml of ethanol
  11. 11
    أخرىan m.p. of 61-62° C. (lit. 62° C.)
  12. 12
    أخرىwere obtained

الإجراء التجريبي

A reaction mixture composed of 21.40 g (95.3 mmol) of 98% 4-iodophenol, 12.19 g (95.3 mmol) of 99% benzyl chloride, 20.73 g (150 mmol) of potassium carbonate and 250 ml of acetone was heated to reflux temperature and heated to boiling for 30 hours. After cooling to room temperature, the reaction mixture was filtered. The filtrate was concentrated and then cooled in an ice bath, in the course of which a solid precipitated out. This was removed by means of a blue-band filter and then dried. The crude product (23.22 g) was recrystallized from 70 ml of ethanol. 17.20 g (58% of theory) of colorless microcrystals having an m.p. of 61-62° C. (lit. 62° C.) were obtained.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08029919B2uspto-grants-2011_10