Sodium Hydroxide → 2,6-Bis[(4-azidophenyl)methylidene]-4-methoxycyclohexan-1-one

HRID 1285113

Reaktionsgleichung

Reaktionsgleichung von HRID 1285113
[CH3:1][O:2][CH:3]1[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1.[N:10]([C:13]1[CH:20]=[CH:19][C:16]([CH:17]=O)=[CH:15][CH:14]=1)=[N+:11]=[N-:12].[OH-].[Na+]>C(O)C.O>[N:10]([C:13]1[CH:20]=[CH:19][C:16]([CH:17]=[C:7]2[CH2:8][CH:3]([O:2][CH3:1])[CH2:4][C:5](=[CH:17][C:16]3[CH:19]=[CH:20][C:13]([N:10]=[N+:11]=[N-:12])=[CH:14][CH:15]=3)[C:6]2=[O:9])=[CH:15][CH:14]=1)=[N+:11]=[N-:12]

Komponenten

6

Edukt 3

HCID 14798Sodium HydroxideHCID 903854-AzidobenzaldehydeHCID 5350284-Methoxycyclohexanone

Produkt 1

HCID 538953902,6-Bis[(4-azidophenyl)methylidene]-4-methoxycyclohexan-1-oneAusbeute 15,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

In 100 ml of ethanol were dissolved 10 g of 4-methoxycyclohexanone and 30 g of para-azidobenzaldehyde, after which a solution of 1 g of sodium hydroxide in 1 ml of water was added, and the resulting mixture was subjected to reaction in a brown flask at room temperature for 2 days. The crystals formed were separated by suction filtration, washed with ethanol, and then recrystallized from methyl Cellosolve to obtain 4.7 g of yellow crystals having a decomposition point of 145° to 150° C. (differential thermal analysis, the rate of heating: 5° C./min).

Aufarbeitung

  1. customthe resulting mixture was subjected to reaction in a brown flask at room temperature for 2 days
  2. customThe crystals formed
  3. customwere separated by suction filtration
  4. washwashed with ethanol
  5. customrecrystallized from methyl Cellosolve

Quellen und Nachweise

ORD-Eintrag
ord-7ad50651cff748829c9552d823d95db3
Quelldatensatz
uspto-grants-1986_01
Patentnummer
US04565767

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