Reaktionsgleichung
[O:1]=C1C2C(C=CN=2)=NC1=O.C1C=CC2SC3C=CC=CC=3NC=2C=1.[CH3:25][C:26]12[CH2:35][CH2:34][CH2:33][CH2:32][CH:31]1[C:30](=[O:36])[O:29][C:27]2=[O:28].C(OCCO)(=O)C(C)=C>C1C(Cl)=CC=C(Cl)C=1>[CH3:25][C:26]1([CH2:35][CH2:34][CH2:33][CH2:32][CH:31]1[C:30]([OH:29])=[O:36])[C:27]([OH:1])=[O:28]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
2.35 g (0.005 mol) of the diketopyrrolopyrrole of the formula XIX (Example 6) and 30 ml of dichlorobenzene are placed under nitrogen in a sulfonating flask, 5.0 mg (0.05 mmol) of thiodiphenylamine are added, and the mixture is heated with stirring at 110°-115° C. 3.17 g (0.010 mol) of the methyl-hexahydrophthalic acid derivative (isomer mixture) of the formula ##STR43## (obtained by generally known methods from methylhexahydrophthalic anhydride and hydroxyethyl methacrylate) are added dropwise with vigorous stirring over the course of 15 minutes to the clear orange-red solution, stirring is continued for about 2 hours at 110°-115° C., and then the mixture is cooled to room temperature. The clear dark red solution is washed in a separating funnel 3 times with 20 ml of 5% sodium hydroxide solution and 2 times with 30 ml of deionized water, and the organic phase is dried over MgSO4 ·H2O, filtered and concentrated to dryness under a high vacuum. The resulting product is recrystallized from 30 ml of ethanol, to give 3.05 g (81.3% of theory) of a crystalline product of the formula ##STR44## with a melting point of 69.6° C.
Aufarbeitung
- temperaturethe mixture is heated
Quellen und Nachweise
- ORD-Eintrag
- ord-e0bf8a2d57cf41bf8a4cedf5cd1cbd45
- Quelldatensatz
- uspto-grants-1998_12
- Patentnummer
- US05847156
Verknüpfte Notizen
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