Dichloromethane → HCID 72721606, Verbindung
Reaktionsgleichung
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[CH:4][N:3]=1.Cl.[NH2:10][C:11]1[C:16]([CH3:17])=[CH:15][C:14](/[CH:18]=[CH:19]/[C:20]#[N:21])=[CH:13][C:12]=1[CH3:22].C(N(CC)C(C)C)(C)C.C(Cl)Cl>O>[Cl:1][C:2]1[N:7]=[C:6]([NH:10][C:11]2[C:16]([CH3:17])=[CH:15][C:14](/[CH:18]=[CH:19]/[C:20]#[N:21])=[CH:13][C:12]=2[CH3:22])[CH:5]=[CH:4][N:3]=1Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 145 °C
Versuchsvorschrift
To a mixture of 2,4-dichloropyrimidine (5 gm) and (E)-3-(4-amino-3,5-dimethylphenyl)acrylonitrile hydrochloride (6 gm) was added N,N-diisopropylethylamine (60 ml) under stirring. The mixture was then heated to 140 to 150° C. and stirred for 55 to 60 hours. The solution was then cooled to room temperature and the solvent was distilled off under reduced pressure to provide a residual solid. To the residual solid was added methylene chloride (300 ml) and water (250 ml). The reaction mass was stirred for 30 minutes at room temperature and then the layers were separated. The organic layer was dried with sodium sulfate and then concentrates to provide 5 gm of (E)-3-(4-(2-chloropyrimidin-4-ylamino)-3,5-dimethylphenyl)acrylonitrile.
Aufarbeitung
- stirringstirred for 55 to 60 hours
- temperatureThe solution was then cooled to room temperature
- distillationthe solvent was distilled off under reduced pressure
- customto provide a residual solid
- stirringThe reaction mass was stirred for 30 minutes at room temperature
- customthe layers were separated
- dry with materialThe organic layer was dried with sodium sulfate
Quellen und Nachweise
- ORD-Eintrag
- ord-eb67069a221843d4b293353d46220758
- Quelldatensatz
- uspto-grants-2015_09
- Patentnummer
- US09139535B2
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