Sodium Acetate → HCID 18177433, Verbindung

HRID 428190Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 428190
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[O:9][CH2:8][CH:7]([CH2:13][C:14]#[N:15])[CH2:6]2.[C:16]([O-])(=[O:18])[CH3:17].[Na+].[H][H]>[Ni].C(OC(=O)C)(=O)C.C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[O:9][CH2:8][CH:7]([CH2:13][CH2:14][NH:15][C:16](=[O:18])[CH3:17])[CH2:6]2

Komponenten

7

Edukt 3

HCID 517045Sodium AcetateHCID 18177464HCID 18177464, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 18177433HCID 18177433, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 935NickelKatalysatorHCID 7918Acetic AnhydrideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

0.812 g (4 mmol) of the nitrile obtained in Step C is added to a suspension of 0.35 g (6 mmol) of Raney nickel and 0.5 g (6 mmol) of sodium acetate in 40 ml of acetic anhydride. The reaction medium is then subjected to hydrogen pressure of 50 psi at a temperature of 50° C. for 5 hours. After cooling of the mixture, the salts are filtered off and the filtrate is concentrated under reduced pressure. The residue obtained is then taken up in ethyl acetate; the organic phase is then washed with a saturated solution of sodium hydrogen carbonate. After drying over magnesium sulphate and filtration, the solvent is evaporated in vacuo. Chromatography on a silica column (eluant:AcOEt) results in the title amide in the form of a white solid.

Aufarbeitung

  1. temperatureAfter cooling of the mixture
  2. filtrationthe salts are filtered off
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. customThe residue obtained
  5. washthe organic phase is then washed with a saturated solution of sodium hydrogen carbonate
  6. dry with materialAfter drying over magnesium sulphate and filtration
  7. customthe solvent is evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-6798afa66463453593beef7c30e6e9a9
Quelldatensatz
uspto-grants-2001_11
Patentnummer
US06313160B1

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