Реакция #2026

ord-987cbce73ecd44fa89c19bbd9f39470c

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas heated
  2. 2
    Температураat reflux temperature for 20 h
  3. 3
    ТемператураAfter the mixture was cooled in the refrigerator, crystals
  4. 4
    Другоеwere collected
  5. 5
    ДругоеThe crude product was repeatedly recrystallized from water-ethanol
  6. 6
    ДругоеThe trace amount of inorganic salts was removed
  7. 7
    workup.ADDITIONby treating the aqueous solution with a small amount of silver(I) oxide and barium hydroxide
  8. 8
    workup.ADDITIONtreated three times with Amberlite-120 (sodium form) ion-exchange resin
  9. 9
    ДругоеAfter removal of the water
  10. 10
    Другоеthe product was recrystallized from water-ethanol

Методика

A mixture of 1,2-dibromoethane (37.6 g, 0.20 mol) and sodium sulfite (63.0 g, 0.5 mol) in water (225 mL) was heated at reflux temperature for 20 h. After the mixture was cooled in the refrigerator, crystals were collected. The crude product was repeatedly recrystallized from water-ethanol. The trace amount of inorganic salts was removed by treating the aqueous solution with a small amount of silver(I) oxide and barium hydroxide. The basic solution was neutralized with Amberlite-120 ion-exchange resin and treated three times with Amberlite-120 (sodium form) ion-exchange resin. After removal of the water, the product was recrystallized from water-ethanol to afford the title compound (30.5 g).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05728375uspto-grants-1998_03