Stannous Chloride → HCID 146733, Verbindung

HRID 1354567Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1354567
[N+:1]([C:4]1[CH:25]=[CH:24][C:7]([CH:8]=[CH:9][C:10]2[C:11]3[C:16]([N:17]=[C:18]4[C:23]=2[CH:22]=[CH:21][CH:20]=[CH:19]4)=[CH:15][CH:14]=[CH:13][CH:12]=3)=[CH:6][CH:5]=1)([O-])=O.[Sn](Cl)Cl>C(OCC)(=O)C.C(O)C>[NH2:1][C:4]1[CH:25]=[CH:24][C:7]([CH:8]=[CH:9][C:10]2[C:23]3[C:18]([N:17]=[C:16]4[C:11]=2[CH:12]=[CH:13][CH:14]=[CH:15]4)=[CH:19][CH:20]=[CH:21][CH:22]=3)=[CH:6][CH:5]=1

Komponenten

5

Edukt 2

HCID 24479Stannous ChlorideHCID 730989559-(4-Nitrostyryl)acridine2×

Produkt 1

HCID 146733HCID 146733, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

The 9-(4-nitrostyryl)acridine product (2.86 g, 10.0 mmol) is dissolved in ethyl acetate (250 ml) and then brought to reflux. A solution of tin(II) chloride dehydrate (9.0 g, 40 mmol) in hot ethanol (150 ml) is cooled and added to the solution of 9-(4-nitrostyryl)acridine. The mixture is reacted under reflux and with stirring for 5 hours. After cooling, the 9-(4-aminostyryl)acridine precipitates and is isolated by filtration under vacuum. The filtrate is dried by evaporation and taken up in water (500 ml) with stirring. The solution is basified (pH 13–14) with a sodium hydroxide solution. The 9-(4-aminostyryl)acridine fraction previously isolated, which contains a high proportion of tin salt, is also basified. The 9-(4-aminostyryl)acridine is separated by filtration, washed with water and dried. It is sufficiently pure for the following step.

Aufarbeitung

  1. temperatureto reflux
  2. customThe mixture is reacted
  3. temperatureunder reflux
  4. temperatureAfter cooling
  5. customthe 9-(4-aminostyryl)acridine precipitates
  6. customis isolated by filtration under vacuum
  7. customThe filtrate is dried by evaporation
  8. stirringwith stirring

Quellen und Nachweise

ORD-Eintrag
ord-5699240b52254bce8e67decfb3b46acb
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07223865B2

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