Reacción #2026

ord-987cbce73ecd44fa89c19bbd9f39470c

Ecuación de reacción

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

Reactantes

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

Reactivos

Ninguno

Disolventes

O
water

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas heated
  2. 2
    Temperaturaat reflux temperature for 20 h
  3. 3
    TemperaturaAfter the mixture was cooled in the refrigerator, crystals
  4. 4
    Otrowere collected
  5. 5
    OtroThe crude product was repeatedly recrystallized from water-ethanol
  6. 6
    OtroThe 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
    OtroAfter removal of the water
  10. 10
    Otrothe product was recrystallized from water-ethanol

Procedimiento

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).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05728375uspto-grants-1998_03