Potassium Carbonate → HCID 21553923, Verbindung

HRID 267793

Reaktionsgleichung

Reaktionsgleichung von HRID 267793
[Cl:1][C:2]1[CH:9]=[C:6]([CH:7]=[O:8])[C:5]([OH:10])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH:18]([CH3:21])[C:19]#[N:20]>CC(C)=O>[Cl:1][C:2]1[CH:9]=[C:6]([C:5]([O:10][CH:18]([C:19]#[N:20])[CH3:21])=[CH:4][CH:3]=1)[CH:7]=[O:8]

Komponenten

5

Edukt 3

HCID 11430Potassium Carbonate2×HCID 124815-Chloro-salicylaldehydeHCID 5192252-Chloropropionitrile2×

Produkt 1

HCID 21553923HCID 21553923, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

A mixture of 5-chlorosalicylaldehyde (78 g., 0.5 mole), finely powdered anhydrous potassium carbonate (103.5 g., 0.75 mole) and acetone (500 ml.) is stirred under reflux and 2-chloropropionitrile (33.6 g., 0.375 mole) is added over a period of about 5 minutes. The mixture is heated under reflux for 1.5 hours and then treated with potassium carbonate (34.5 g., 0.25 mole) followed by more 2-chloropropionitrile (11.2 g., 0.125 mole). Heating and stirring are continued for 31/2 hours, after which the reaction mixture is filtered and the filter-cake washed with acetone. Evaporation of the combined filtrate gives 3-chloro-6-(1-cyanoethoxy)-benzaldehyde which is recrystallized from aqueous methanol.

Aufarbeitung

  1. temperatureunder reflux
  2. temperatureThe mixture is heated
  3. temperatureunder reflux for 1.5 hours
  4. temperatureHeating
  5. stirringstirring
  6. custom2 hours
  7. filtrationafter which the reaction mixture is filtered
  8. washthe filter-cake washed with acetone
  9. customEvaporation of the combined filtrate

Quellen und Nachweise

ORD-Eintrag
ord-7a6b98e1ac1041ad9fec417b3c3d37b2
Quelldatensatz
uspto-grants-1976_03
Patentnummer
US03944560

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