Oxalic Acid → HCID 11680498, Verbindung

HRID 2185671Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2185671
[CH3:1][NH:2][C:3]([C@@H:5]1[CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[N:6]1[C:14](=[O:29])[C@@H:15]([NH:18]C(OCC1C=CC=CC=1)=O)[CH2:16][CH3:17])=[O:4].C(O)(=O)C(O)=O>CO.[Pd]>[CH3:1][NH:2][C:3]([C@@H:5]1[CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[N:6]1[C:14](=[O:29])[C@@H:15]([NH2:18])[CH2:16][CH3:17])=[O:4]

Komponenten

5

Edukt 2

HCID 971Oxalic AcidHCID 69969204HCID 69969204, Verbindung

Produkt 1

HCID 11680498HCID 11680498, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

2.15 g (5.44 mmol) of the compound obtained in step d) are dissolved in 200 ml of methanol and 0.85 g of activated 10% palladium-on-charcoal (wet) is added. The reaction mixture is hydrogenated at 60 psi for 3 hours. The solution is filtered and 1.3 equivalents (0.64 g) of oxalic acid (7.07 mmol) are added and the solution is then concentrated under vacuum. Ethanol is added, followed by ether (1:50 ratio) and a crystallized product is obtained. After filtration and washing with diethyl ether, the solid is dried under vacuum for 24 hours over P2O5 at 35° C. The desired product is obtained.

Aufarbeitung

  1. filtrationThe solution is filtered
  2. concentrationthe solution is then concentrated under vacuum
  3. additionEthanol is added
  4. customa crystallized product is obtained
  5. filtrationAfter filtration
  6. washwashing with diethyl ether
  7. dry with materialthe solid is dried under vacuum for 24 hours over P2O5 at 35° C

Quellen und Nachweise

ORD-Eintrag
ord-6c6aea63739c4bd5b87b711aaff6c1fb
Quelldatensatz
uspto-grants-2002_06
Patentnummer
US06403561B1

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