Ethylenediamine → HCID 68601740, Verbindung

HRID 1640518Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1640518
Cl[C:2]1[CH:3]=[CH:4][N:5]=[C:6]2[C:11]=1[N:10]=[C:9]([O:12][CH3:13])[CH:8]=[CH:7]2.[CH2:14]([NH2:17])[CH2:15][NH2:16]>C(Cl)Cl>[CH3:13][O:12][C:9]1[N:10]=[C:11]2[C:6](=[CH:7][CH:8]=1)[N:5]=[CH:4][CH:3]=[C:2]2[NH:16][CH2:15][CH2:14][NH2:17]

Komponenten

4

Edukt 2

HCID 3301EthylenediamineHCID 222443958-Chloro-2-methoxy-1,5-naphthyridine

Produkt 1

HCID 68601740HCID 68601740, VerbindungAusbeute 51 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 8-chloro-2-methoxy-1,5-naphthyridine (1.71 g, 8.81 mmol) and ethylenediamine (1.18 mL, 2 eq.) was heated slowly to 80° C. over 1 h and subsequently up to 100° C. for 2 h. After cooling to rt, the yellow solution was taken in DCM and successively washed with NaHCO3. The aq. layer was back extracted with DCM (3 times) and the combined org. layers were concentrated to afford the title intermediate as a pale yellow oil (0.98 g, 51% yield).

Aufarbeitung

  1. temperatureAfter cooling to rt
  2. washsuccessively washed with NaHCO3
  3. extractionThe aq. layer was back extracted with DCM (3 times)
  4. concentrationlayers were concentrated

Quellen und Nachweise

ORD-Eintrag
ord-973d97214c57474cac618b88ec5152b3
Quelldatensatz
uspto-grants-2012_02
Patentnummer
US08114867B2

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