반응 #2026

반응 방정식

1,2-dibromoethane

sodium sulfite

→

title compound

수율 65.1%

Sodium ethane-1,2-disulfonate

수율 65.1%

용매

water

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux temperature for 20 h
3. 3
   온도After the mixture was cooled in the refrigerator, crystals
4. 4
   기타were collected
5. 5
   기타The crude product was repeatedly recrystallized from water-ethanol
6. 6
   기타The 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
   기타After removal of the water
10. 10
    기타the product was recrystallized from water-ethanol

실험 절차

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).

출처