تفاعل #81684

ord-13be94cbd57447c6bb28e782fbef3cb4

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05618975uspto-grants-1997_04