Water → HCID 178471932, Verbindung

HRID 36714Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 36714
[Cl:1][C:2]1[C:19]([F:20])=[C:18]([Cl:21])[CH:17]=[C:16]([F:22])[C:3]=1[C:4]([C:6](=[CH:12]OCC)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5].[F:23][C:24]1[CH:30]=[C:29]([F:31])[CH:28]=[CH:27][C:25]=1[NH2:26].O>C(O)C>[Cl:1][C:2]1[C:19]([F:20])=[C:18]([Cl:21])[CH:17]=[C:16]([F:22])[C:3]=1[C:4]([C:6](=[CH:12][NH:26][C:25]1[CH:27]=[CH:28][C:29]([F:31])=[CH:30][C:24]=1[F:23])[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5]

Komponenten

5

Edukt 3

HCID 962WaterHCID 97092,4-DifluoroanilineHCID 53750212Ethyl 2-(2,4-dichloro-3,6-difluorobenzoyl)-3-ethoxyacrylate

Produkt 1

HCID 178471932HCID 178471932, VerbindungAusbeute 92,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

35.3 g of ethyl 2-(2,4-dichloro-3,6-difluorobenzoyl)-3-ethoxyacrylate are dissolved in 120 ml of ethanol, and 12.9 g of 2,4-difluoroaniline are added dropwise, while cooling with ice. The mixture is stirred at room temperature for 1.5 hours, 120 ml of water are added, while cooling, and the precipitate is filtered off with suction, rinsed with ethanol/H2O (1:1) and dried. 40.5 g of ethyl 2-(2,4-dichloro-3,6-difluorobenzoyl)-3-(2,4-difluorophenylamino)acrylate are obtained, melting point: 84°-86° C.

Aufarbeitung

  1. temperaturewhile cooling with ice
  2. temperaturewhile cooling
  3. filtrationthe precipitate is filtered off with suction
  4. washrinsed with ethanol/H2O (1:1)
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-184b6a62583644f5b7de2687c702ee1b
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05416096

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