3-Aminobenzenesulfonic acid → 2-Amino-5-methoxybenzenesulfonic acid

HRID 2210619

반응식

HRID 2210619 반응식
[NH2:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=CC(S(O)(=O)=O)=CC=2O)[C:3]=1[S:17]([OH:20])(=[O:19])=[O:18].FC1N=NN=C(F)C=1F.[C:30](=[O:33])([O-])[O-].[Na+].[Na+].S(O)(=O)(C1C=CC=C(N)C=1)=O>O>[NH2:1][C:2]1[CH:11]=[CH:10][C:9]([O:33][CH3:30])=[CH:4][C:3]=1[S:17]([OH:20])(=[O:18])=[O:19]

참가 물질

6

반응물 4

HCID 84743-Aminobenzenesulfonic acidHCID 10340Sodium Carbonate2회HCID 810242-Amino-5-hydroxynaphthalene-1,7-disulphonic acidHCID 138991444,5,6-Trifluoro-1,2,3-triazine

생성물 1

HCID 832602-Amino-5-methoxybenzenesulfonic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

31.9 g of 2-amino-5-hydroxy-naphthalene-1,7-disulphonic acid are dissolved in 400 ml of water to give a neutral solution. 300 g of ice are then added, and 8.8 ml of trifluorotriazine are allowed to run in, a pH of 4.0-4.5 being maintained with 15% strength sodium carbonate solution. The mixture is subsequently stirred for 5 minutes, a neutral solution of 17.3 g of m-sulphanilic acid is then added, and a pH of 5.0-5.5 is maintained with 15% strength sodium carbonate solution. During the acylation, the temperature is allowed to rise to 15°-20°. A diazo compound obtained by the customary route by diazotisation of 20.3 g of 1-amino-4-methoxy-benzene-2-sulphonic acid is added to the resulting solution of the reaction product of the formula ##STR17## at 5°-10°, the pH simultaneously being kept at pH 7.0-7.5 by sprinkling in sodium bicarbonate. When the coupling has ended, the dyestuff of the formula ##STR18## is salted out, filtered off with suction, dried and ground. The red dyestuff powder dissolves readily in water and dyes cotton a clear scarlet (colour code number 6) by a process customary for reactive dyestuffs.

후처리

  1. customto give a neutral solution
  2. customto rise to 15°-20°

출처 및 근거

ORD 기록
ord-63c74d09286d44088e75b436244f8053
출처 데이터셋
uspto-grants-1995_10
특허 번호
US05459246

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