Réaction #2026

ord-987cbce73ecd44fa89c19bbd9f39470c

Équation de réaction

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

Réactifs

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

Réactifs

Aucun

Solvants

O
water

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurewas heated
  2. 2
    Températureat reflux temperature for 20 h
  3. 3
    TempératureAfter the mixture was cooled in the refrigerator, crystals
  4. 4
    Autrewere collected
  5. 5
    AutreThe crude product was repeatedly recrystallized from water-ethanol
  6. 6
    AutreThe 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
    AutreAfter removal of the water
  10. 10
    Autrethe product was recrystallized from water-ethanol

Mode opératoire

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).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05728375uspto-grants-1998_03