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Sodium Hydroxide → HCID 178526872, Verbindung

HRID 610480
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 610480
[OH-:1].[Na+].CC(O)(C)CN[C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[N:10]2[N:17]=[N:18][N:19]=[C:9]2[C:8]=1[N+:20]([O-:22])=[O:21]>O>[N+:20]([C:8]1[C:9]2[N:10]([N:17]=[N:18][N:19]=2)[C:11]2[C:16]([C:7]=1[OH:1])=[CH:15][CH:14]=[CH:13][CH:12]=2)([O-:22])=[O:21]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 154897582-Methyl-[(4-nitro-5-tetrazolo[1,5-a]quinolinyl)amino]-2-propanol

Produkt 1

HCID 178526872HCID 178526872, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Aqueous sodium hydroxide (30 g of 50%) was added to a suspension of 2-methyl-[(4-nitro-5-tetrazolo[1,5-a]quinolinyl)amino]-2-propanol (34.0 g, 0.1125 mole, Example 3) in water (500 mL). The mixture was heated on a steam bath and the solid dissolved rapidly. The solution was heated for about 30 minutes and then upon stirring a solid began to precipitate. The mixture was made acidic with 6N hydrochloric acid. The resulting solid was isolated by filtration; washed in succession with water, ethanol and ether; then dried under vacuum at 100° C. to provide 23.2 g of crude product as a pale yellow/green solid. A sample (3.2 g) was recrystallized initially from methanol/dichloromethane and then from toluene to provide 4-nitrotetrazolo[1,5-a]quinolin-5-ol. Analysis: Calculated for C9H5N5O3 : % C, 46.76; % H, 2.18; % N, 30.29; Found: % C, 46.85; % H, 2.23; % N, 29.91.

Aufarbeitung

  1. temperatureThe mixture was heated on a steam bath
  2. dissolutionthe solid dissolved rapidly
  3. temperatureThe solution was heated for about 30 minutes
  4. customto precipitate
  5. customThe resulting solid was isolated by filtration
  6. washwashed in succession with water, ethanol and ether
  7. customthen dried under vacuum at 100° C.
  8. customto provide 23.2 g of crude product as a pale yellow/green solid
  9. customA sample (3.2 g) was recrystallized initially from methanol/dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-46d8180e7bb04403adc3b55f52f232f2
Quelldatensatz
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05998619

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