Ammonium Chloride → HCID 178422376, Verbindung

HRID 1439463Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1439463
[C:1]([C:3]1[C:4](=[O:14])[O:5][C:6]2[C:11]([C:12]=1[CH3:13])=[CH:10][CH:9]=[CH:8][CH:7]=2)#[N:2].[N-:15]=[N+:16]=[N-:17].[Na+].[Cl-].[NH4+]>CN(C=O)C>[CH3:13][C:12]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[O:5][C:4](=[O:14])[C:3]=1[C:1]1[NH:17][N:16]=[N:15][N:2]=1

Komponenten

5

Edukt 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 2311463-Cyano-4-methylcoumarin

Produkt 1

HCID 178422376HCID 178422376, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 3-cyano-4-methyl coumarin (7.94 g; 0.043 mole) in cimethylformamide (DMF) (45 ml) was added to a mixture of sodium azide (2.92 g; 0.044 mole) and ammonium chloride (2.36 g; 0.044 mole) and the stirred mixture heated on a steam bath for 24 hours. After removal of the solvent under reduced pressure, water (100 ml) was added and the solid filtered off. Acidification of the filtrate, and further aqueous extracts, afforded the title compound; m.p. (EtOH) 213°-4° C (Found: C, 57.58; H, 3.51; N, 24.41; C11H8N4O2 requires; C, 57.89; H, 3.53; N, 24.55%).

Aufarbeitung

  1. temperaturethe stirred mixture heated on a steam bath for 24 hours
  2. customAfter removal of the solvent under reduced pressure, water (100 ml)
  3. additionwas added
  4. filtrationthe solid filtered off

Quellen und Nachweise

ORD-Eintrag
ord-0ee7cc680d8a4bf292d524c40ab7193d
Quelldatensatz
uspto-grants-1977_11
Patentnummer
US04059704

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