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Hydrochloric Acid → HCID 20135876, Verbindung

HRID 484896
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 484896
[CH2:1]([N:3]([CH2:31][CH3:32])[CH2:4][CH2:5][CH2:6][N:7]1[C:15]2[C:10](=[CH:11][C:12]([N+:19]([O-])=O)=[CH:13][C:14]=2[N+:16]([O-])=O)[C:9]([NH:22][CH2:23][CH2:24][CH2:25][N:26]([CH2:29][CH3:30])[CH2:27][CH3:28])=[N:8]1)[CH3:2].CO.O.Cl>[Fe].C(Cl)(Cl)Cl>[CH2:31]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][CH2:6][N:7]1[C:15]2[C:10](=[CH:11][C:12]([NH2:19])=[CH:13][C:14]=2[NH2:16])[C:9]([NH:22][CH2:23][CH2:24][CH2:25][N:26]([CH2:27][CH3:28])[CH2:29][CH3:30])=[N:8]1)[CH3:32]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 962WaterHCID 20135767HCID 20135767, Verbindung

Produkt 1

HCID 20135876HCID 20135876, VerbindungAusbeute 23,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925Iron
Katalysator
HCID 6212ChloroformLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A mixture consisting of 12.0 g of the 1-(3-diethylaminopropyl)-3-(3-diethylaminopropylamino)-5,7-dinitroindazole, 18 g of iron powder, 60 ml of methyl alcohol, 30 ml of water and 3 ml of hydrochloric acid was stirred for 1.5 hours at 70° C. After cooling, the mixture was filtered, and the pH of the filtrate was adjusted to 11 with an aqueous potassium carbonate solution. The filtrate was extracted three times with 50 ml of ethyl acetate, and the ethyl acetate layer was washed with water. The layer was dried over anhydrous sodium sulfate, and ethyl acetate was removed under reduced pressure. The residue thus obtained was subjected to an alumina-column chromatography (alumina: 200 g) using chloroform as the developing solvent to give 2.46 g of 1-(3-diethylaminopropyl)-3-(3-diethylaminopropylamino)-5,7-diaminoindazole having the following analytical values in a yield of 23%.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationthe mixture was filtered
  3. extractionThe filtrate was extracted three times with 50 ml of ethyl acetate
  4. washthe ethyl acetate layer was washed with water
  5. dry with materialThe layer was dried over anhydrous sodium sulfate, and ethyl acetate
  6. customwas removed under reduced pressure
  7. customThe residue thus obtained

Quellen und Nachweise

ORD-Eintrag
ord-b5efbfb913a5466185b4fe07023694ee
Quelldatensatz
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04533731

Notizen zur Reaktion

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