تفاعل #2026

ord-987cbce73ecd44fa89c19bbd9f39470c

معادلة التفاعل

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

المتفاعلات

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

الكواشف

لا شيء

المذيبات

O
water

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةat reflux temperature for 20 h
  3. 3
    درجة الحرارةAfter the mixture was cooled in the refrigerator, crystals
  4. 4
    أخرىwere collected
  5. 5
    أخرىThe crude product was repeatedly recrystallized from water-ethanol
  6. 6
    أخرىThe 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
    أخرىAfter removal of the water
  10. 10
    أخرىthe product was recrystallized from water-ethanol

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05728375uspto-grants-1998_03