1,2-Dibromoethane → Sodium 1,2-Ethanedisulfonate

HRID 1740680

反応式

HRID 1740680 の反応式
Br[CH2:2][CH2:3]Br.[S:5]([O-:8])([O-:7])=[O:6].[Na+:9].[Na+]>O>[CH2:2]([S:5]([O-:8])(=[O:7])=[O:6])[CH2:3][S:5]([O-:8])(=[O:7])=[O:6].[Na+:9].[Na+:9]

参加物

4

反応物 2

HCID 78391,2-DibromoethaneHCID 24437Sodium Sulfite

生成物 1

HCID 79220Sodium 1,2-Ethanedisulfonate収率 65.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

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).

後処理

  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

出典と根拠

ORDレコード
ord-f856d704d4a245c9a29ec4e346026a69
出典データセット
uspto-grants-1999_10
特許番号
US05972328

関連ノート

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