Sodium Carbonate → 8-(5-Nitro-o-toluenesulfonamido)-1,3,6-naphthalenetrisulfonic acid

HRID 903841

Reaktionsgleichung

Reaktionsgleichung von HRID 903841
[NH2:1][C:2]1[CH:3]=[C:4]([S:20]([OH:23])(=[O:22])=[O:21])[CH:5]=[C:6]2[C:11]=1[C:10]([S:12]([OH:15])(=[O:14])=[O:13])=[CH:9][C:8]([S:16]([OH:19])(=[O:18])=[O:17])=[CH:7]2.C1C(N=NC2C(=O)N(C3C=CC(S([O-])(=O)=O)=CC=3)N=C2C([O-])=O)=CC=C(S([O-])(=O)=O)C=1.[Na+].[Na+].[Na+].C(=O)([O-])[O-].[Na+].[Na+].[N+:64]([C:67]1[CH:72]=[C:71]([CH3:73])[C:70]([S:74](Cl)(=[O:76])=[O:75])=[CH:69][CH:68]=1)([O-:66])=[O:65]>O>[N+:64]([C:67]1[CH:72]=[C:71]([CH3:73])[C:70]([S:74]([NH:1][C:2]2[CH:3]=[C:4]([S:20]([OH:23])(=[O:22])=[O:21])[CH:5]=[C:6]3[C:11]=2[C:10]([S:12]([OH:15])(=[O:14])=[O:13])=[CH:9][C:8]([S:16]([OH:19])(=[O:17])=[O:18])=[CH:7]3)(=[O:76])=[O:75])=[CH:69][CH:68]=1)([O-:66])=[O:65]

Komponenten

6

Edukt 4

HCID 10340Sodium Carbonate2×HCID 649518-Aminonaphthalene-1,3,6-trisulfonic acidHCID 888695-Nitrotoluene-2-sulfonyl chlorideHCID 164825Tartrazine

Produkt 1

HCID 867365448-(5-Nitro-o-toluenesulfonamido)-1,3,6-naphthalenetrisulfonic acidAusbeute 841,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 17.0 g of 8-amino-1,3,6-naphthalenetrisulfonic acid, trisodium salt, 17.5 g of the preceding compound and 7.8 g of anhydrous sodium carbonate in 210 ml of water is stirred at room temperature for 18 hours, then an additional 0.5 g of sodium carbonate and 1.0 g of 5-nitro-o-toluenesulfonyl chloride is added and stirring is continued for 18 hours longer. The reaction mixture is evaporated and 100 ml of water is added with stirring. The mixture is filtered and 900 ml of absolute ethanol is added to the filtrate with stirring. The mixture is stirred for 2 hours, then the precipitate is collected and is washed with ethanol and ether and is dried to yield 20.8 g of 8-(5-nitro-o-toluenesulfonamido)-1,3,6-naphthalenetrisulfonic acid, trisodium salt.

Aufarbeitung

  1. stirringstirring
  2. waitis continued for 18 hours
  3. customThe reaction mixture is evaporated
  4. addition100 ml of water is added
  5. stirringwith stirring
  6. filtrationThe mixture is filtered
  7. addition900 ml of absolute ethanol is added to the filtrate
  8. stirringwith stirring
  9. stirringThe mixture is stirred for 2 hours
  10. customthe precipitate is collected
  11. washis washed with ethanol and ether
  12. customis dried

Quellen und Nachweise

ORD-Eintrag
ord-3cdb8d02234447f681aa082b05c07bf9
Quelldatensatz
uspto-grants-1980_10
Patentnummer
US04229372

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