Reaktionsgleichung
[C:1]1([S:17]([O-:20])(=O)=[O:18])[C:14]2[C:13](=[O:15])[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[C:6](=[O:16])[C:5]=2[CH:4]=[CH:3][CH:2]=1.[Na+].O=P(Cl)(Cl)[Cl:24].S1(CCCC1)(=O)=O>C(#N)C>[Cl:24][S:17]([C:1]1[C:14]2[C:13](=[O:15])[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[C:6](=[O:16])[C:5]=2[CH:4]=[CH:3][CH:2]=1)(=[O:20])=[O:18]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 110 °C
Versuchsvorschrift
Sodium anthraquinone-1-sulfonate (50.0 g) was combined with POCl3 (31 mL) and a 1:2 (v/v) mixture of sulfolane (100 mL) and acetonitrile (200 mL). The mixture was stirred and heated to 110° C. under a nitrogen atmosphere for 44 hours. The mixture was allowed to cool to room temperature and was then further cooled in a refrigerator. The mixture was filtered and the filtrate was poured onto ice in a beaker and this mixture was stirred for 1 hour. The brown precipitate was filtered, washed with deionized water, dried in air and then further dried overnight in a vacuum oven at 45° C. and less than 1 mmHg pressure to give 12.08 g of the product as a brown solid.
Aufarbeitung
- temperatureto cool to room temperature
- temperaturewas then further cooled in a refrigerator
- filtrationThe mixture was filtered
- additionthe filtrate was poured onto ice in a beaker
- stirringthis mixture was stirred for 1 hour
- filtrationThe brown precipitate was filtered
- washwashed with deionized water
- customdried in air
- customfurther dried overnight in a vacuum oven at 45° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-e893ef734055413fb2485a5f1980b686
- Quelldatensatz
- uspto-grants-2008_02
- Patentnummer
- US07329692B2
Verknüpfte Notizen
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