Methanol → HCID 178430148, Verbindung

HRID 896968

Reaktionsgleichung

Reaktionsgleichung von HRID 896968
C=CC1C=CC=CC=1.C(O)(=O)C(C)=C.CO.[OH-].[K+].O.[CH3:20][C:21]1[C:26]([NH:27][C:28]2[C:33]3[C:34]([Cl:41])=[C:35]([Cl:40])[C:36]([Cl:39])=[C:37]([Cl:38])[C:32]=3[C:30](=[O:31])[N:29]=2)=[CH:25][CH:24]=[CH:23][C:22]=1[NH:42][C:43]1[C:48]2[C:49]([Cl:56])=[C:50]([Cl:55])[C:51]([Cl:54])=[C:52]([Cl:53])[C:47]=2[C:45](=[O:46])[N:44]=1>CS(C)=O.C1(=O)C2C(=CC=CC=2)CN1>[C:30]1(=[O:31])[C:32]2[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=2)[CH2:28][NH:29]1.[CH3:20][C:21]1[C:22]([NH:42][C:43]2[C:48]3[C:49]([Cl:56])=[C:50]([Cl:55])[C:51]([Cl:54])=[C:52]([Cl:53])[C:47]=3[C:45](=[O:46])[N:44]=2)=[CH:23][CH:24]=[CH:25][C:26]=1[NH:27][C:28]1[C:33]2[C:34]([Cl:41])=[C:35]([Cl:40])[C:36]([Cl:39])=[C:37]([Cl:38])[C:32]=2[C:30](=[O:31])[N:29]=1

Komponenten

8

Edukt 5

HCID 887MethanolHCID 962Water2×HCID 14797Potassium HydroxideHCID 1657302-Methylprop-2-enoic acid;styreneHCID 178430147HCID 178430147, Verbindung4×

Produkt 1

HCID 178430148HCID 178430148, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 10199PhthalimidineLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

As a dispersing agent having a crosslinkable functional group, 9.5 parts of a styrene/methacrylic acid copolymer (acid value: 290; molecular weight: 15,000) were dissolved in 80 parts of dimethyl sulfoxide, and 10 parts of an isoindolinone pigment (C.I. Pigment Yellow 109) were suspended in the resultant solution in a flask at 25° C. under an air atmosphere. A 30% methanol solution of potassium hydroxide was then added dropwise little by little to dissolve the isoindolinone pigment. After the pigment solution was stirred for 3 hours, p-phenylene-bis(ethyl)carbodiimide as a crosslinking agent was added to and dissolved in the pigment solution in a proportion of 1 part per 10 parts of the pigment, and the resultant solution was quickly poured into ion-exchanged water (400 parts of ion-exchanged water per 10 parts of the pigment; 0° C.) stirred by an impellor type agitating blade (800 rpm), purged with nitrogen and cooled and temperature-maintained by means of 2 system dispensers (manufactured by Musashi Engineering K.K.; needle internal diameter: 0.57 mm; delivery pressure: 4.0 kgf/cm2) to obtain an aqueous dispersion of isoindolinone-pigment-containing particles having an average particle diameter of 35.6 nm. This aqueous dispersion was transferred to a reaction vessel equipped with a mantle heater, cooling tower, stirrer and thermometer, this system was purged with nitrogen with stirring at 300 rpm, 10% hydrochloric acid was added dropwise to adjust the pH of the reaction mixture to 4.75. After continuing the reaction for additional 5 hours, the resultant aggregates were filtered under reduced pressure through a membrane filter (holding particle diameter: 0.45 am) and washed 3 times with 500 ml of ion-exchanged water to obtain paste of an aqueous dispersion of the isoindolinone-pigment-containing particles desalted and desolvated.

Aufarbeitung

  1. stirringagitating blade (800 rpm)
  2. custompurged with nitrogen
  3. temperaturecooled
  4. temperaturetemperature-maintained by means of 2 system dispensers (manufactured by Musashi Engineering K.K.; needle internal diameter: 0.57 mm; delivery pressure: 4.0 kgf/cm2)

Quellen und Nachweise

ORD-Eintrag
ord-6a2ba8da322842529034ea6afa4759b0
Quelldatensatz
uspto-grants-2005_07
Patentnummer
US06921433B2

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