Ethanone, 1-(3,4-dichlorophenyl)- → 1-(3,4-Dichlorophenyl)-3-(dimethylamino)prop-2-en-1-one

HRID 231530

Reaktionsgleichung

Reaktionsgleichung von HRID 231530
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[C:6]([Cl:11])[CH:5]=1)=[O:3].CO[CH:14](OC)[N:15]([CH3:17])[CH3:16]>>[Cl:11][C:6]1[CH:5]=[C:4]([C:2](=[O:3])[CH:1]=[CH:14][N:15]([CH3:17])[CH3:16])[CH:9]=[CH:8][C:7]=1[Cl:10]

Komponenten

3

Edukt 2

HCID 75841Ethanone, 1-(3,4-dichlorophenyl)-HCID 78373Dimethylformamide dimethyl acetal

Produkt 1

HCID 28051561-(3,4-Dichlorophenyl)-3-(dimethylamino)prop-2-en-1-one

Versuchsvorschrift

A mixture of 50.0 g of 3,4-dichloroacetophenone and 75 ml of N,N-dimethylformamide dimethyl acetal was heated under reflux for 6 hours, then allowed to cool for 16 hours. The crystalline precipitate was collected by filtration, washed with hexane and dried. The addition of hexane to the above filtrate precipitated some additional product which was collected by filtration. The precipitates were combined, washed with hexane and dried in vacuo to give 55.0 g of 3',4'-dichloro-3-dimethylaminoacrylophenone as bright yellow crystals.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 6 hours
  3. temperatureto cool for 16 hours
  4. filtrationThe crystalline precipitate was collected by filtration
  5. washwashed with hexane
  6. customdried
  7. additionThe addition of hexane to the above filtrate
  8. customprecipitated some additional product which
  9. filtrationwas collected by filtration
  10. washwashed with hexane
  11. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-bb1052c824674d639b76eec8fbf3e767
Quelldatensatz
uspto-grants-1989_07
Patentnummer
US04847256

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