Reacción #81684

ord-13be94cbd57447c6bb28e782fbef3cb4

Disolventes

Condiciones de reacción

Temperatura
0°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

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

Procedimiento

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).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05618975uspto-grants-1997_04