1,3-Diethyl 2-oxopropanedioate → HCID 68476438, Verbindung

HRID 1942135Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1942135
[NH2:1][C:2]1[C:3]([NH:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[N:4][CH:5]=[CH:6][CH:7]=1.O=[C:16]([C:22](OCC)=[O:23])[C:17]([O:19][CH2:20][CH3:21])=[O:18]>C(O)C>[O:23]=[C:22]1[N:8]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:3]2[N:4]=[CH:5][CH:6]=[CH:7][C:2]=2[N:1]=[C:16]1[C:17]([O:19][CH2:20][CH3:21])=[O:18]

Komponenten

4

Edukt 2

HCID 691051,3-Diethyl 2-oxopropanedioateHCID 106790912-N-phenylpyridine-2,3-diamine

Produkt 1

HCID 68476438HCID 68476438, VerbindungAusbeute 58 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

11.68 g (63 mmol) of 3-amino-2-anilinopyridine was dissolved in ethanol (150 mL), and 12.07 g (69 mmol) of diethyl ketomalonate was added thereto. The mixture was heated to reflux for 4 hours while stirring. After confirming the completion of the reaction, the reaction solution was cooled to room temperature, and the solvent was distilled off under reduced pressure. The residue thus obtained was washed using diisopropyl ether, to obtain 10.74 g (yield: 58%) of ethyl 3-oxo-4-phenyl-3,4-dihydropyrido[2,3-b]pyrazine-2-carboxylate as pale yellow crystals.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 4 hours
  3. customthe completion of the reaction
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue thus obtained
  6. washwas washed

Quellen und Nachweise

ORD-Eintrag
ord-4adfd40748164249b3bdbde6abb660c9
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08389523B2

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