Potassium Iodide → 2-Iodobenzene-1-sulfonamide

HRID 53406

反応式

HRID 53406 の反応式
N[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8]([NH2:11])(=[O:10])=[O:9].N([O-])=O.[Na+].[I-:16].[K+]>OS(O)(=O)=O.O>[I:16][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8]([NH2:11])(=[O:10])=[O:9]

参加物

6

反応物 3

HCID 4875Potassium IodideHCID 728942-AminobenzenesulfonamideHCID 23668193Sodium Nitrite

生成物 1

HCID 28248922-Iodobenzene-1-sulfonamide収率 69.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒3 回HCID 1118Sulfuric Acid溶媒

反応条件

温度
0 °C

実験手順

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).

後処理

  1. customto give a clear solution
  2. customwithout exceeding 5°-6° C
  3. stirringthe obtained red mixture is stirred for 18 hours
  4. filtrationthe obtained precipitate is filtered
  5. washwashed several times in water
  6. dissolutionThe obtained solid is dissolved in ethyl acetate
  7. washwashed once with 0.2N sodiumthiosulfate solution and twice with water
  8. customevaporated to dryness

出典と根拠

ORDレコード
ord-13be94cbd57447c6bb28e782fbef3cb4
出典データセット
uspto-grants-1997_04
特許番号
US05618975

関連ノート

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