Acetic Acid → HCID 178418570, Verbindung

HRID 5241

Reaktionsgleichung

Reaktionsgleichung von HRID 5241
[NH2:1][C:2]1[C:3]([NH:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[C:26](=[NH:34])[NH:27][O:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])=[CH:16][CH:15]=2)=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].[CH2:35]([O:37][C:38](OCC)(OCC)OCC)[CH3:36].C(O)(=O)C>O1CCOCC1>[CH2:35]([O:37][C:38]1[N:12]([CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[C:26](=[NH:34])[NH:27][O:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])=[CH:16][CH:15]=2)[C:3]2[C:4]([C:5]([O:7][CH3:8])=[O:6])=[CH:9][CH:10]=[CH:11][C:2]=2[N:1]=1)[CH3:36]

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 66213Tetraethyl orthocarbonateHCID 178418614HCID 178418614, Verbindung

Produkt 1

HCID 178418570HCID 178418570, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

The pale brown syrup (8.58 g) obtained in Example (57a) was dissolved in dioxane (20 ml). To the solution were added tetraethoxymethane (8.64 g) and acetic acid (1.56 g). The mixture was stirred for 2 hours at 100° C. The reaction mixture was concentrated to dryness. The residue was crystallized from ethyl acetate (50 ml). Resulting crystalline precipitates were collected by filtration to obtain the title compound.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated to dryness
  2. customThe residue was crystallized from ethyl acetate (50 ml)
  3. customResulting crystalline precipitates
  4. filtrationwere collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-e6e2a39337d44b93874b16d5ca671d7a
Quelldatensatz
uspto-grants-1993_09
Patentnummer
US05243054

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