Sodium Bicarbonate → 1,3-Diazaazulene

HRID 1199345

Reaktionsgleichung

Reaktionsgleichung von HRID 1199345
S[C:2]1[N:3]=[C:4]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=[C:5]2[N:6]=1.C(=O)(O)[O-].[Na+]>[N+]([O-])(O)=O>[N:3]1[C:4]2=[CH:11][CH:10]=[CH:9][CH:8]=[CH:7][C:5]2=[N:6][CH:2]=1

Komponenten

4

Edukt 2

HCID 516892Sodium BicarbonateHCID 178527782HCID 178527782, Verbindung

Produkt 1

HCID 6380091,3-Diazaazulene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 944Nitric AcidLösungsmittel

Versuchsvorschrift

With reference to Journal of the American Chemical Society, vol. 76, pages 3352 and 3353 (1954) 23 g of 2-mercaptocycloheptimidazole as synthesized in Synthetic example 1(b) was added to 210 ml of 10% nitric acid, and stirred with heating to the inner temperature of 80° to 90° C. for one hour. The reaction solution was neutralized with sodium bicarbonate and extracted with chloroform (250 ml×2). The chloroform layer was dried over anhydrous sodium sulfate and concentrated to 50 ml under reduced pressure, and then 200 ml of hexane was added. Deposited crystals were collected by filtration and dried.

Aufarbeitung

  1. temperaturewith heating to the inner temperature of 80° to 90° C. for one hour
  2. extractionextracted with chloroform (250 ml×2)
  3. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated to 50 ml under reduced pressure
  5. addition200 ml of hexane was added
  6. filtrationDeposited crystals were collected by filtration
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-b4a41319e01b46608a12a0adb449755c
Quelldatensatz
uspto-grants-1990_02
Patentnummer
US04900648

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