4-Sulfophthalic acid → Phthaloperinone sulphochloride

HRID 2398070

Reaktionsgleichung

Reaktionsgleichung von HRID 2398070
[S:1]([C:5]1[C:6](=[O:25])[C:7]2[N:8]3[C:16]([N:17]=[C:18]4[C:24]=2[C:22]([CH:23]=1)=[CH:21][CH:20]=[CH:19]4)=[C:15]1[C:10]([CH:11]=[CH:12][CH:13]=[CH:14]1)=[CH:9]3)([OH:4])(=[O:3])=[O:2].S(C1C=C(C(O)=O)C(=CC=1)C(O)=O)(O)(=O)=O.C1C=C(N)C2C(N)=CC=CC=2C=1.P(Cl)(Cl)([Cl:56])=O>CN1CCCC1=O.C1(C)C(C)=CC=CC=1>[C:6]1(=[O:25])[C:7]2=[C:24]3[C:18](=[N:17][C:16]4[N:8]2[CH:9]=[C:10]2[C:15]=4[CH:14]=[CH:13][CH:12]=[CH:11]2)[CH:19]=[CH:20][CH:21]=[C:22]3[CH:23]=[CH:5]1.[S:1]([Cl:56])([OH:4])(=[O:3])=[O:2]

Komponenten

7

Edukt 4

HCID 69624-Sulfophthalic acidHCID 24813Phosphorus oxychlorideHCID 680671,8-DiaminonaphthaleneHCID 21434658Sulphophthaloperinone

Produkt 1

HCID 86734752Phthaloperinone sulphochlorideAusbeute 91,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 7237O-XyleneLösungsmittelHCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

11.5 g of sulphophthaloperinone, prepared from 4-sulphophthalic acid and 1,8-naphthylenediamine in N-methylpyrrolidone, are suspended in 100 ml of xylene. 9.2 g of phosphorus oxychloride are added and the mixture is heated to 80° C for 6 - 7 hours, whilst stirring. 25 - 30 ml of xylene are then distilled off under reduced pressure and after cooling the reaction product which has precipitated is filtered off and the residue is rinsed with petroleum ether. 11.6 g of phthaloperinone-sulphochloride are obtained.

Aufarbeitung

  1. distillation25 - 30 ml of xylene are then distilled off under reduced pressure
  2. temperatureafter cooling the reaction product which
  3. customhas precipitated
  4. filtrationis filtered off
  5. washthe residue is rinsed with petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-81a6fe1d67a5465a8a61445368ca5662
Quelldatensatz
uspto-grants-1977_05
Patentnummer
US04024144

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