Hydrochloric Acid → HCID 178515425, Verbindung

HRID 26661

Reaktionsgleichung

Reaktionsgleichung von HRID 26661
[Cl-].[Al+3].[Cl-].[Cl-].[O:5]=[C:6]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[O:9][CH:8]=[C:7]1[C:16]#[N:17].[N-:18]=[N+:19]=[N-:20].[Na+].Cl>O1CCCC1>[NH:18]1[C:16]([C:7]2[C:6](=[O:5])[C:11]3[C:10](=[CH:15][CH:14]=[CH:13][CH:12]=3)[O:9][CH:8]=2)=[N:17][N:20]=[N:19]1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 33557Sodium AzideHCID 5212984-Oxo-4H-chromene-3-carbonitrileHCID 6451240Aluminum(III) Chloride

Produkt 1

HCID 178515425HCID 178515425, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To 100 volume parts of dry tetrahydrofuran are added 4.28 parts of comminuted anhydrous aluminum chloride, 2.50 parts of 4-oxo-4H-1-benzopyran-3-carbonitrile and 4.18 parts of sodium azide in this order and, the whole mixture is refluxed under stirring for 23 hours. Then, to the resulting mixture 35 volume parts of 15 weight% hydrochloric acid are added, followed by distilling off tetrahydrofuran under reduced pressure. The resulting solid residue is recovered by filtration and recrystallized from dimethylformamide. This procedure yields 3-(1H-tetrazol-5-yl) chromone as colorless hairy needles. Melting point: 284°-285° C.(decomp. with foaming).

Aufarbeitung

  1. temperaturethe whole mixture is refluxed
  2. distillationby distilling off tetrahydrofuran under reduced pressure
  3. filtrationThe resulting solid residue is recovered by filtration
  4. customrecrystallized from dimethylformamide

Quellen und Nachweise

ORD-Eintrag
ord-7b96c81ffadc464497b8bf34f0ecad9d
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04151180

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