H acid → 2-Aminobenzenesulfonic acid

HRID 1632148

반응식

HRID 1632148 반응식
N[C:2]1[C:11]2[C:6](=CC(S(O)(=O)=O)=CC=2O)[CH:5]=[C:4]([S:17]([OH:20])(=[O:19])=[O:18])[CH:3]=1.[N:21]1C(F)=NC(F)=NC=1F.C(=O)([O-])[O-].[Na+].[Na+].NC1C=CC=C2C=1C=CC(S(O)(=O)=O)=C2.N([O-])=O.[Na+]>O.Cl>[NH2:21][C:5]1[CH:6]=[CH:11][CH:2]=[CH:3][C:4]=1[S:17]([OH:20])(=[O:19])=[O:18]

참가 물질

8

반응물 5

HCID 7009H acidHCID 84081,6-Cleve's acidHCID 10340Sodium Carbonate2회HCID 12664Cyanuric fluorideHCID 23668193Sodium Nitrite

생성물 1

HCID 69262-Aminobenzenesulfonic acid

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매2회

실험 절차

34.1 g of 1-amino-8-hydroxynaphthalene-3,6-disulphonic acid are dissolved in 400 ml of water at pH 5.5. After cooling the solution to 0°-5°, 9.2 ml of cyanuric fluoride are added dropwise in the course of 10 minutes, and during this the pH value in the solution is kept at 4.0-4.5 by adding 20% strength sodium carbonate solution dropwise. The solution is subsequently stirred at this pH value and at 0°-5° for 1/2 an hour and 24.5 g of 5-aminonaphthalene-2-sulphonic acid are then added. The ph value of the solution kept at 5.5-6.0 with sodium carbonate solution and the temperature is gradually increased to 20° in the course of 2 hours. After the condensation reaction has ended, the mixture is again cooled to 0°-10° and the suspension of a diazonium compound which has been obtained from 18.4 g of 2-aminobenzenesulphonic acid in 200 ml of water and 30 ml of concentrated hydrochloric acid with 54 ml of 2N sodium nitrite solution in the manner shown in the Example is now added.

후처리

  1. temperatureAfter cooling the solution to 0°-5°
  2. additionare then added
  3. temperaturethe temperature is gradually increased to 20° in the course of 2 hours
  4. customAfter the condensation reaction
  5. temperaturethe mixture is again cooled to 0°-10°

출처 및 근거

ORD 기록
ord-7d55753b748a459c86dd42ddeb34b343
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04474697

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