Acetic Anhydride → HCID 12669250, Verbindung

HRID 430508

Reaktionsgleichung

Reaktionsgleichung von HRID 430508
[C:1]([NH:4][C:5]1[CH:9]=[CH:8][S:7][C:6]=1[C:10]([OH:12])=[O:11])(=O)[CH3:2].C([O-])(=O)C.[Na+].C(OC(=O)C)(=O)C>O1CCOCC1>[CH3:2][C:1]1[O:12][C:10](=[O:11])[C:6]2[S:7][CH:8]=[CH:9][C:5]=2[N:4]=1

Komponenten

5

Edukt 3

HCID 7918Acetic AnhydrideHCID 517045Sodium AcetateHCID 28075793-Acetamidothiophene-2-carboxylic acid

Produkt 1

HCID 12669250HCID 12669250, VerbindungAusbeute 119,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a mixture of 3-acetamidothiophene-2-carboxylic acid (15.1 g, 75.67 mmol) and sodium acetate (6.45 g, 78.6 mmol) in dioxane (200 mL) was added acetic anhydride (71 mL, 75.7 mmol). The reaction was refluxed 2 hours, cooled to ambient temperature and partitioned between chloroform and water. Phases were separated and the aqueous layer was extracted with chloroform. The combined organic phase was washed with water and brine, dried over magnesiuym sulfate and concentrated to leave 15.1 g of 2-methyl-thieno[3,2-d][1,3]oxazin-4-one as a brown oil which slowly solidified.

Aufarbeitung

  1. temperatureThe reaction was refluxed 2 hours
  2. custompartitioned between chloroform and water
  3. customPhases were separated
  4. extractionthe aqueous layer was extracted with chloroform
  5. washThe combined organic phase was washed with water and brine
  6. dry with materialdried over magnesiuym sulfate
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-82c2df153c004ea5b5d5c17398b9629d
Quelldatensatz
uspto-grants-2001_11
Patentnummer
US06323208B1

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