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Hydrochloric Acid → Perylene

HRID 1413330
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1413330
C(O)(=O)CCCCCCCCCCCCCCCCC.[C:21]1(C(O)=O)[C:38]2=[C:39]3[C:28]([C:29]4[C:40]5[C:33](=[CH:34][CH:35]=[CH:36][C:37]2=5)[CH:32]=[CH:31][CH:30]=4)=[CH:27][CH:26]=[C:25](C(O)=O)[C:24]3=[C:23](C(O)=O)[C:22]=1C(O)=O.C(O)(=O)CCCCCCCCCCCCCCCCC.C(N)CCCCCCCCCCCCCCCCC.Cl>[K].C1(C(O)=O)C2=C3C(C4C5C(=CC=CC2=5)C=CC=4)=CC=C(C(O)=O)C3=C(C(O)=O)C=1C(O)=O.[OH-].[K+].C(O)(C)C>[CH:36]1[C:37]2=[C:40]3[C:29]([C:28]4[C:39]5[C:24](=[CH:23][CH:22]=[CH:21][C:38]2=5)[CH:25]=[CH:26][CH:27]=4)=[CH:30][CH:31]=[CH:32][C:33]3=[CH:34][CH:35]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 4

HCID 313Hydrochloric AcidHCID 5281Stearic AcidHCID 15793OctadecylamineHCID 86737471HCID 86737471, Verbindung

Produkt 1

HCID 9142Perylene

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 3776IsopropanolLösungsmittel
HCID 14797Potassium HydroxideLösungsmittel2×
HCID 5462222PotassiumLösungsmittel
HCID 19063515Perylene-1,2,3,4-tetracarboxylic acidLösungsmittel

Versuchsvorschrift

27.4 parts of crude perylenetetracarboxylic dianhydride in the form of the potassium salt of perylenetetracarboxylic acid are dissolved in aqueous potassium hydroxide solution as described in Example 1. To this solution are added 2 parts of stearic acid, dissolved in 60 parts by volume of 1% potassium hydroxide solution. With stirring, the alkaline perylenetetracarboxylic acid/stearic acid solution is added dropwise in the course of 15 minutes at 60° C. to a suspension consisting of 1.4 parts of MgCl2.6H2O, 0.7 parts of stearylamine, 35 parts by volume of about 37% aqueous hydrochloric acid and 60 parts by volume of isopropanol. The formation of the anhydride imide is brought to completion by stirring the acid suspension for 31/2 hours at reflux temperature. The red pigment suspension is then filtered at about 70° C. The filter cake is washed neutral with cold water and dried in a vacuum cabinet at 80° C., affording 29.8 parts of a perylene pigment with properties as good as those of the pigment of Example 1.

Aufarbeitung

  1. stirringby stirring the acid suspension for 31/2 hours
  2. temperatureat reflux temperature
  3. filtrationThe red pigment suspension is then filtered at about 70° C
  4. washThe filter cake is washed neutral with cold water
  5. customdried in a vacuum cabinet at 80° C.

Quellen und Nachweise

ORD-Eintrag
ord-87b70f3364c44a2c930935bdf9f06233
Quelldatensatz
uspto-grants-1981_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04250079

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