Reaktion #350554

ord-80089ade5a8c47c7aaa1d9487a404892

Reaktionsgleichung

BrCCBr
1,2-dibromoethane
O=S([O-])[O-].[Na+].[Na+]
sodium sulfite
→
O=S(=O)([O-])CCS(=O)(=O)[O-].[Na+].[Na+]
title compound
Ausbeute 65.1%
O=S(=O)([O-])CCS(=O)(=O)[O-].[Na+].[Na+]
Sodium ethane-1,2-disulfonate
Ausbeute 65.1%

Edukte

BrCCBr
1,2-dibromoethane
O=S([O-])[O-].[Na+].[Na+]
sodium sulfite

Reagenzien

Keine

Lösungsmittel

O
water

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturat reflux temperature for 20 h
  3. 3
    TemperaturAfter the mixture was cooled in the refrigerator, crystals
  4. 4
    Sonstigewere collected
  5. 5
    SonstigeThe crude product was repeatedly recrystallized from water-ethanol
  6. 6
    SonstigeThe 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
    SonstigeAfter removal of the water
  10. 10
    Sonstigethe product was recrystallized from water-ethanol

Vorschrift

A mixture of 1,2-dibromoethane (37.6 g, 0.20 tool) 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).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05643562uspto-grants-1997_07