Ethanol → HCID 178482634, Verbindung

HRID 1282981Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1282981
[Cl-].[CH3:2][N:3]([CH3:28])[C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[C:14]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[S+:13]=[C:12]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH:11]=2)=[CH:6][CH:5]=1.C(O)C.[CH3:32][N:33]([CH3:51])[C:34]1[CH:39]=[CH:38][C:37]([N:40]=[N:41][C:42]2[CH:50]=[CH:49][C:45]([C:46]([O-:48])=[O:47])=[CH:44][CH:43]=2)=[CH:36][CH:35]=1.[Na+]>O>[CH3:32][N:33]([CH3:51])[C:34]1[CH:35]=[CH:36][C:37]([N:40]=[N:41][C:42]2[CH:50]=[CH:49][C:45]([C:46]([O-:48])=[O:47])=[CH:44][CH:43]=2)=[CH:38][CH:39]=1.[CH3:2][N:3]([CH3:28])[C:4]1[CH:5]=[CH:6][C:7]([C:10]2[CH:11]=[C:12]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[S+:13]=[C:14]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH:15]=2)=[CH:8][CH:9]=1

Komponenten

5

Edukt 3

HCID 702EthanolHCID 23674498Benzoic acid, 4-(2-(4-(dimethylamino)phenyl)diazenyl)-, sodium salt (1:1)HCID 178482633HCID 178482633, Verbindung

Produkt 1

HCID 178482634HCID 178482634, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

To a hot solution composed of 4.04 g. 4-(4-dimethylaminophenyl)-2,6-diphenylthiapyrylium chloride, 200 mls. water, and 50 mls. ethanol, was added in one portion a solution of sodium 4-(4-dimethylaminophenylazo)benzoate, 3.0 g., in hot water, 150 mls. There was immediate formation of a fine, dark-brown precipitate. The reaction mixture was quickly chilled in ice, and then filtered. The filtrate was a clear, deep orange. The solid was washed with cold water until the washings were only weakly orange. The solid was sucked dry and then a portion of it was dissolved in boiling acetonitrile, filtered hot, and evaporated down. The crystalline solid that came down on cooling the concentrated solution was filtered off and dried in vacuo. This solid was found to contain the above-noted thiapyrylium-azo dye salt.

Aufarbeitung

  1. temperatureThe reaction mixture was quickly chilled in ice
  2. filtrationfiltered
  3. washThe solid was washed with cold water until the washings
  4. customThe solid was sucked dry
  5. dissolutiona portion of it was dissolved
  6. filtrationfiltered hot
  7. customevaporated down
  8. temperatureon cooling the concentrated solution
  9. filtrationwas filtered off
  10. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-d5846a98ca5d46b092763da42d65d79d
Quelldatensatz
uspto-grants-1976_08
Patentnummer
US03973962

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