Reaktion #81684

Reaktionsgleichung

potassium iodide

2-aminobenzene sulfonamide

NaNO2

→

light yellow compound

Ausbeute 69.5%

2-iodobenzene sulfonamide

Ausbeute 69.5%

Lösungsmittel

H2O

H2O

H2SO4

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto give a clear solution
2. 2
   Sonstigewithout exceeding 5°-6° C
3. 3
   workup.STIRRINGthe obtained red mixture is stirred for 18 hours
4. 4
   Filtrationthe obtained precipitate is filtered
5. 5
   Waschenwashed several times in water
6. 6
   workup.DISSOLUTIONThe obtained solid is dissolved in ethyl acetate
7. 7
   Waschenwashed once with 0.2N sodiumthiosulfate solution and twice with water
8. 8
   Sonstigeevaporated to dryness

Vorschrift

2-aminobenzene sulfonamide (3.5 g) in conc. H2SO4, 98% (25 ml) are heated at 60° to give a clear solution. 20 g of ice is then added and the solution is cooled to 0° C. NaNO2 (1.45 g) in water (4 ml) is added dropwise very carefully without exceeding 5°-6° C. The reaction mixture is stirred at 5°-6° C. for 3 hours. A solution of potassium iodide (3.75 g) in H2O (25 ml) is then introduced dropwise and the obtained red mixture is stirred for 18 hours. H2O (50 ml) is added and the obtained precipitate is filtered, washed several times in water. The obtained solid is dissolved in ethyl acetate, washed once with 0.2N sodiumthiosulfate solution and twice with water, evaporated to dryness to give 4 g of a light yellow compound (62% yield).

Quelle