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Acetic Anhydride → HCID 14881376, Verbindung

HRID 2352620
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2352620
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].OCC[N:11]1[C:16]([CH3:17])=[C:15]([CH3:18])[N:14]=[C:13]([CH3:19])[C:12]1=[O:20]>N1C=CC=CC=1>[C:5]([O:4][CH2:1][CH2:2][N:11]1[C:16]([CH3:17])=[C:15]([CH3:18])[N:14]=[C:13]([CH3:19])[C:12]1=[O:20])(=[O:7])[CH3:6]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 7918Acetic AnhydrideHCID 147735301-(2-Hydroxyethyl)-3,5,6-trimethylpyrazin-2-one

Produkt 1

HCID 14881376HCID 14881376, VerbindungAusbeute 51,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

Acetic anhydride (2 ml) was added under ice-cooling to compound 026 (0.91 g, 5 mM) dissolved in pyridine (10 ml), and stirred at room temperature for 1.5 hours. The reaction mixture was concentrated in vacuo and dilute aqueous K2CO3 was added thereto, the resultant mixture being extracted three times with chloroform. The extract was dried with anhydrous magnesium sulfate and concentrated in vacuo. The residue was charged on a column of silica-gel (Florisil, 60 g) packed with benzene and eluted with benzene-ethyl acetate (5:1) to obtain compound 061 (0.58 g, yield: 51.8%).

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated in vacuo and dilute aqueous K2CO3
  2. additionwas added
  3. extractionthe resultant mixture being extracted three times with chloroform
  4. dry with materialThe extract was dried with anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. additionThe residue was charged on a column of silica-gel (Florisil, 60 g)
  7. washeluted with benzene-ethyl acetate (5:1)

Quellen und Nachweise

ORD-Eintrag
ord-c4f556085d164398b8df5a59597ca538
Quelldatensatz
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04877877

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