Aniline → 2-Aminobenzenesulfonic acid

HRID 1073354

反応式

HRID 1073354 の反応式
[S:1]([O-:5])([OH:4])(=[O:3])=[O:2].[NH3+:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[NH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>[OH-].[Na+]>[NH2:6][C:7]1[C:8]([S:1]([OH:5])(=[O:3])=[O:2])=[CH:9][CH:10]=[CH:11][CH:12]=1.[NH2:13][C:14]1[C:19]([S:1]([OH:4])(=[O:3])=[O:2])=[CH:18][C:17]([S:1]([OH:5])(=[O:4])=[O:3])=[CH:16][CH:15]=1

参加物

5

反応物 2

HCID 6115AnilineHCID 69584289Anilinium hydrogen sulphate

生成物 2

HCID 69262-Aminobenzenesulfonic acid収率 0.7%HCID 673044-Amino-1,3-benzenedisulfonic acid収率 0.02%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

439.7 g of powdered anilinium hydrogensulphate were heated for 7 hours at 200° C. in a closed autoclave. After cooling, the autoclave was opened and the solid was dissolved in 1N NaOH (pH 7.2), deposited aniline was separated off, residual aniline was removed by extraction with methylene chloride (2×100 ml) and the aqueous phase was evaporated to dryness. The analysis of the powdery product showed a yield of p-sulphanilic acid Na salt of 68.5%, based on employed aniline. 0.7% of aniline-2-sulphonic acid and 0.02% of aniline-2,4-disulphonic acid were formed.

後処理

  1. temperatureAfter cooling
  2. customwas separated off
  3. customresidual aniline was removed by extraction with methylene chloride (2×100 ml)
  4. customthe aqueous phase was evaporated to dryness

出典と根拠

ORDレコード
ord-9ab542f1b293423bb2ec286125977690
出典データセット
uspto-grants-1990_11
特許番号
US04968835

関連ノート

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