Aniline → 2-Aminobenzenesulfonic acid

HRID 1073354

반응식

HRID 1073354 반응식
[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

참가 물질

5

반응물 2

HCID 6115AnilineHCID 69584289Anilinium hydrogen sulphate

생성물 2

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

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9ab542f1b293423bb2ec286125977690
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04968835

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