Реакция #1747866

ord-eee27b9e4fe147dd8e55086696d664d8

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas heated
  2. 2
    Температураto reflux temperature
  3. 3
    Температураheated
  4. 4
    Фильтрацияthe reaction mixture was filtered
  5. 5
    КонцентрированиеThe filtrate was concentrated
  6. 6
    Температураcooled in an ice bath, in the course of which a solid
  7. 7
    Другоеprecipitated out
  8. 8
    ДругоеThis was removed by means of a blue-band filter
  9. 9
    Другоеdried
  10. 10
    ДругоеThe crude product (23.22 g) was recrystallized from 70 ml of ethanol
  11. 11
    Другоеan m.p. of 61-62° C. (lit. 62° C.)
  12. 12
    Другоеwere obtained

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08029919B2uspto-grants-2011_10