1,3,6-Naphthalenetrisulfonic acid, 8-amino-, sodium salt (1:?) → 8-(3-Nitro-2-sulfobenzamido)-1,3,6-naphthalene trisulfonic acid tetrasodium salt

HRID 66034

Reaktionsgleichung

Reaktionsgleichung von HRID 66034
[Na+:1].[Na+].[Na+].[NH2:4][C:5]1[CH:6]=[C:7]([S:23]([O-:26])(=[O:25])=[O:24])[CH:8]=[C:9]2[C:14]=1[C:13]([S:15]([O-:18])(=[O:17])=[O:16])=[CH:12][C:11]([S:19]([O-:22])(=[O:21])=[O:20])=[CH:10]2.O.O.O.C([O-])(=O)C.[Na+].[N+](C1C(S(O)(=O)=O)=C(C=CC=1)C([O:43][C:44](=O)[C:45]1[CH:50]=[CH:49][CH:48]=[C:47]([N+:51]([O-:53])=[O:52])[C:46]=1[S:54]([OH:57])(=[O:56])=[O:55])=O)([O-])=O>O>[Na+:1].[Na+:1].[Na+:1].[Na+:1].[N+:51]([C:47]1[C:46]([S:54]([OH:57])(=[O:55])=[O:56])=[C:45]([CH:50]=[CH:49][CH:48]=1)[C:44]([NH:4][C:5]1[CH:6]=[C:7]([S:23]([O-:26])(=[O:25])=[O:24])[CH:8]=[C:9]2[C:14]=1[C:13]([S:15]([O-:18])(=[O:17])=[O:16])=[CH:12][C:11]([S:19]([O-:22])(=[O:20])=[O:21])=[CH:10]2)=[O:43])([O-:53])=[O:52]

Komponenten

5

Edukt 3

HCID 1018991,3,6-Naphthalenetrisulfonic acid, 8-amino-, sodium salt (1:?)HCID 151200803-Nitrosulfobenzoic anhydrideHCID 23665404Sodium Acetate Trihydrate

Produkt 1

HCID 1317113728-(3-Nitro-2-sulfobenzamido)-1,3,6-naphthalene trisulfonic acid tetrasodium saltAusbeute 353,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

To a solution of 20.0 g of 8-amino-1,3,6-naphthalenetrisulfonic acid trisodium salt and 8.75 g of sodium acetate trihydrate in 180 ml of water at room temperature is added 12.0 g of 3-nitrosulfobenzoic anhydride with stirring. A 400 ml portion of water is added. The mixture is stirred at room temperature for 21/2 hours and then filtered. The filtrate is cooled, acidified with 2-3 ml of concentrated hydrochloric acid an diluted with ethanol. The pink solid is collected by filtration, washed with 85% ethanol, ether and dried. The filtrate is concentrated to a low volume and diluted with ethanol giving a second crop which is collected and combined with the first crop giving a total of 27.6 g of 8-(3-nitro-2-sulfobenzamido)-1,3,6-naphthalene trisulfonic acid tetrasodium salt.

Aufarbeitung

  1. stirringThe mixture is stirred at room temperature for 21/2 hours
  2. filtrationfiltered
  3. temperatureThe filtrate is cooled
  4. additionan diluted with ethanol
  5. filtrationThe pink solid is collected by filtration
  6. washwashed with 85% ethanol, ether
  7. customdried
  8. concentrationThe filtrate is concentrated to a low volume
  9. additiondiluted with ethanol giving a second crop which
  10. customis collected

Quellen und Nachweise

ORD-Eintrag
ord-8d7f49324533496f98d5befcfa55d907
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04129590

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