反応 #2026

反応方程式

1,2-dibromoethane

sodium sulfite

→

title compound

収率 65.1%

Sodium ethane-1,2-disulfonate

収率 65.1%

溶媒

water

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度at reflux temperature for 20 h
3. 3
   温度After the mixture was cooled in the refrigerator, crystals
4. 4
   その他were collected
5. 5
   その他The crude product was repeatedly recrystallized from water-ethanol
6. 6
   その他The 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
   その他After removal of the water
10. 10
    その他the product was recrystallized from water-ethanol

実験手順

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).

出典