Reaktionsgleichung
C1C2=C3C(C4C5C(=CC=CC2=5)C=CC=4)=CC=C2C(OC(=O)C(=C23)C=1)=O.C1(N)CCCCCCC1.N1C=CN=C1.[CH2:40]([CH:46]([N:53]1[C:75](=[O:76])[C:72]2[C:73]3[C:74]4[C:69](=[CH:70][CH:71]=2)[C:68]2[C:77]5[C:64]([CH:65]=[CH:66][CH:67]=2)=[CH:63][CH:62]=[CH:61][C:60]=5[C:59]=4[CH:58]=[CH:57][C:56]=3[C:54]1=[O:55])[CH2:47][CH2:48][CH2:49]CCC)[CH2:41][CH2:42][CH2:43]CC>>[CH:46]1([N:53]2[C:54](=[O:55])[C:56]3[C:73]4[C:74]5[C:59](=[CH:58][CH:57]=3)[C:60]3[C:77]6[C:64]([CH:63]=[CH:62][CH:61]=3)=[CH:65][CH:66]=[CH:67][C:68]=6[C:69]=5[CH:70]=[CH:71][C:72]=4[C:75]2=[O:76])[CH2:40][CH2:41][CH2:42][CH2:43][CH2:49][CH2:48][CH2:47]1Komponenten
Versuchsvorschrift
300 mg (0.93 mmol) of perylene-3,4-dicarboxylic anhydride are reacted with 1.5 g (2.15 mmol) of cyclooctylamine and 3 g of imidazole under an argon inert atmosphere at 140° C. for 12 h as in 2c, and the reaction product is worked up and dried in a drying cabinet. To remove unreacted starting material, the product is boiled in 10 per cent potassium carbonate solution and washed with hot water until the filtrate run-off is colourless. The brown-red product is dried in a drying cabinet at 120° C. and then recrystallized by extraction with ethanol. Yield 290 mg (72%) of dark-red crystalline powder without solid fluorescence, m.p. 342°-343° C., Rf (CHCl3 /silica gel)=0.78. UV (CHCl3): λmax (ε)=506 nm (32000), 484 (32100), 264 (35200). Fluorescence (CHCl3) λmax (Irel)=511 nm, 542 (1), 573 (sh, 0.51).
Aufarbeitung
- customdried in a drying cabinet
- customTo remove unreacted
- washwashed with hot water until the filtrate
- customThe brown-red product is dried in a drying cabinet at 120° C.
- customrecrystallized by extraction with ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-1460794e95284e0c9c8b2ff2d8d1d4c1
- Quelldatensatz
- uspto-grants-1997_07
- Patentnummer
- US05650513
Verknüpfte Notizen
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