HCID 21875489, Verbindung → HCID 21875359, Verbindung

HRID 966912Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 966912
[N+:1]([C:4]1[C:13]2[N:12]=[CH:11][CH:10]=[N:9][C:8]=2[C:7]([C:14]#[N:15])=[CH:6][CH:5]=1)([O-])=O.[H][H]>C(OCC)(=O)C.C(O)C.[Pd]>[NH2:1][C:4]1[C:13]2[NH:12][CH2:11][CH2:10][NH:9][C:8]=2[C:7]([C:14]#[N:15])=[CH:6][CH:5]=1

Komponenten

6

Edukt 2

HCID 21875489HCID 21875489, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 21875359HCID 21875359, VerbindungAusbeute 92,5 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23938PalladiumKatalysatorHCID 702EthanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Compound 468A (0.037 g, 0.18 mmol) was dissolved in a mixture of ethyl acetate (1.0 mL)/ethanol (1.0 mL) and 10% Pd/C (0.050 g) was added. Hydrogen was then introduced via a balloon. After 2 h, the reaction was purged with nitrogen and filtered through Celite, rinsing with ethyl acetate. Concentration in vacuo gave 0.029 g (90%) of compound 469A as a red oil, which was taken on without further purification. HPLC: 97% at 3.217 min (retention time) (YMC S5 ODS column, 4.6×50 mm, eluting with 10-90% aqueous methanol over 4 min containing 0.2% phosphoric acid, 4 mL/min, monitoring at 220 nm).

Aufarbeitung

  1. additionwas added
  2. customthe reaction was purged with nitrogen
  3. filtrationfiltered through Celite
  4. washrinsing with ethyl acetate
  5. concentrationConcentration in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-ef46af3c1da54f1b96f8364bc4221604
Quelldatensatz
uspto-grants-2005_10
Patentnummer
US06953679B2

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