Diethyl Malonate → HCID 66737111, Verbindung

HRID 2096121Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2096121
[NH2:1][C:2]1[C:7]([CH:8]=O)=[CH:6][C:5]([F:10])=[CH:4][N:3]=1.[C:11](OCC)(=[O:18])[CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14].N1CCCCC1>C(O)C>[F:10][C:5]1[CH:6]=[C:7]2[C:2](=[N:3][CH:4]=1)[NH:1][C:11](=[O:18])[C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:8]2

Komponenten

5

Edukt 3

HCID 7761Diethyl MalonateHCID 8082PiperidineHCID 497615922-Amino-5-fluoro-pyridine-3-carbaldehyde

Produkt 1

HCID 66737111HCID 66737111, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 2-amino-5-fluoropyridine-3-carboxaldehyde (2.80 g), diethyl malonate (6.40 g) and piperidine (0.85 g) in ethanol (50 ml) were heated to reflux with stirring for 18 hours, allowed to cool to ambient temperature then evaporated under reduced pressure. The residual solid obtained was washed with diethyl ether then filtered from solution, and sucked to dryness to give the required product as a pale brown solid, 3.97 g. 1H NMR (CDCl3) δ: ca 11.0 (1H, bs), 9.33 (1H, m), 8.66 (1H, d), 8.42 (1H, s), 7.74 (1H, m), 4.45 (2H, q), 1.44 (3H, t).

Aufarbeitung

  1. temperaturewere heated
  2. temperatureto reflux
  3. customthen evaporated under reduced pressure
  4. customThe residual solid obtained
  5. washwas washed with diethyl ether
  6. filtrationthen filtered from solution

Quellen und Nachweise

ORD-Eintrag
ord-50c3a139f6374b10bab4b5b884e6da04
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08450243B2

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