HRID1930

反应详情

EQUATION

反应方程式

HRID 1930 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux temperature for 20 h
  3. temperatureAfter the mixture was cooled in the refrigerator, crystals
  4. customwere collected
  5. customThe crude product was repeatedly recrystallized from water-ethanol
  6. customThe trace amount of inorganic salts was removed
  7. additionby treating the aqueous solution with a small amount of silver(I) oxide and barium hydroxide
  8. additiontreated three times with Amberlite-120 (sodium form) ion-exchange resin
  9. customAfter removal of the water
  10. customthe product was recrystallized from water-ethanol