Hydrochloric Acid → HCID 178516885, Verbindung

HRID 1704747Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1704747
[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][CH:4]=[C:3]1[O:12][CH2:13][C:14]#[N:15].[N-:16]=[N+:17]=[N-:18].[Na+].[Cl-].[NH4+].Cl>CN(C=O)C.O>[NH:16]1[C:14]([CH2:13][O:12][C:3]2[C:2](=[O:1])[C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=3[O:5][CH:4]=2)=[N:15][N:18]=[N:17]1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 22758704HCID 22758704, Verbindung

Produkt 1

HCID 178516885HCID 178516885, VerbindungAusbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
125 °C

Versuchsvorschrift

A mixture of [(4-oxo-4H-1-benzopyran-3-yl)oxy]acetonitrile (2.0 g, 0.01 mole), sodium azide (0.715 g, 0.011 mole) and ammonium chloride (0.56 g, 0.012 mole) in DMF (10 ml) is heated at 125° C. for 7 hrs. under nitrogen. The reaction is cooled overnight and then poured into excess cold water. The aqueous is acidified with 5N hydrochloric acid and the insoluble product is filtered, washed with fresh water and sucked dry. Recrystallization from absolute ethanol gives beige colored crystals (1.45 g, 60%), mp 194°-196° C.

Aufarbeitung

  1. temperatureThe reaction is cooled overnight
  2. filtrationthe insoluble product is filtered
  3. washwashed with fresh water
  4. customsucked dry
  5. customRecrystallization from absolute ethanol

Quellen und Nachweise

ORD-Eintrag
ord-75ec6efd058a426cadf5e032e2c887db
Quelldatensatz
uspto-grants-1978_11
Patentnummer
US04127669

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