Hydrogen Peroxide → Quinacridone

HRID 357503

Reaktionsgleichung

Reaktionsgleichung von HRID 357503
[CH2:1]1[C:6]2[NH:7][C:8]3[C:13]([C:14](=[O:15])[C:5]=2[CH2:4][C:3]2[NH:16][C:17]4[C:22]([C:23](=[O:24])[C:2]1=2)=[CH:21][CH:20]=[CH:19][CH:18]=4)=[CH:12][CH:11]=[CH:10][CH:9]=3.[OH-].[Na+].[Na+].C1C2C(=O)C3C(=CC=CC=3)C(=O)C=2C=CC=1S([O-])(=O)=O.OO>CO>[CH:20]1[CH:21]=[C:22]2[C:23]([C:2]3[C:3]([NH:16][C:17]2=[CH:18][CH:19]=1)=[CH:4][C:5]1[C:14]([C:13]2[C:8]([NH:7][C:6]=1[CH:1]=3)=[CH:9][CH:10]=[CH:11][CH:12]=2)=[O:15])=[O:24]

Komponenten

6

Edukt 4

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 79973Quino(2,3-b)acridine-7,14-dione, 5,6,12,13-tetrahydro-HCID 23661981Sodium 2-anthraquinonesulfonate

Produkt 1

HCID 13976Quinacridone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A one liter flask equipped with a thermometer, stirrer and condenser is charged with 40 grams 6,13-dihydroquinacridone, 0.1 grams phthalimidomethylquinacridone, 250 ml methanol and 52.8 grams 50% aqueous sodium hydroxide. The mixture is stirred under a slow flow of nitrogen at 50° to 55° C. for one hour generating the corresponding 6,13-dihydroquinacridone-di-sodium salt. 0.6 grams anthraquinone-2-sulfonic acid sodium salt are added and the mixture is heated to reflux temperature. 73.5 grams of an aqueous 16.9% hydrogen peroxide solution are added at a rate of 0.4 ml/minute at reflux temperature under a slow nitrogen flow over 2 hours 40 minutes. The resulting red suspension is further stirred for 1 hour at reflux temperature then filtered at 50°-60° C. The presscake is washed with methanol followed by hot water then dried, yielding a gamma I quinacridone as evidenced by the x-ray diffraction pattern. The gamma-I quinacridone is described in U.S. Pat. No. 3,074,950.

Aufarbeitung

  1. customA one liter flask equipped with a thermometer, stirrer and condenser
  2. temperaturethe mixture is heated
  3. temperatureto reflux temperature
  4. temperatureat reflux temperature under a slow nitrogen flow over 2 hours 40 minutes
  5. stirringThe resulting red suspension is further stirred for 1 hour
  6. temperatureat reflux temperature
  7. filtrationthen filtered at 50°-60° C
  8. washThe presscake is washed with methanol
  9. customthen dried

Quellen und Nachweise

ORD-Eintrag
ord-f1c1fc95e9ca4d60b2b867428607eafe
Quelldatensatz
uspto-grants-1998_11
Patentnummer
US05840901

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