Sodium Acetate → 3-acetyl-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine

HRID 542721Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 542721
Cl.[CH3:2][O:3][C:4]1[CH:14]=[CH:13][C:7]2[CH2:8][CH2:9][NH:10][CH2:11][CH2:12][C:6]=2[CH:5]=1.[C:15]([O-])(=[O:17])[CH3:16].[Na+]>C(OC(=O)C)(=O)C>[C:15]([N:10]1[CH2:9][CH2:8][C:7]2[CH:13]=[CH:14][C:4]([O:3][CH3:2])=[CH:5][C:6]=2[CH2:12][CH2:11]1)(=[O:17])[CH3:16]

Komponenten

4

Edukt 2

HCID 517045Sodium AcetateHCID 212429067-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride

Produkt 1

HCID 138533493-acetyl-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7918Acetic AnhydrideLösungsmittel

Versuchsvorschrift

A mixture of 7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride (4.3 g, 0.02 m) and sodium acetate (3.3 g, 0.04 m) in acetic anhydride (13 ml) was refluxed and stirred for 16 hours, concentrated in vacuo and partitioned between methylene chloride and water. The organic phase was dried with magnesium sulfate, filtered and concentrated in vacuo to give 3-acetyl-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine, m.p. 89°-90°.

Aufarbeitung

  1. temperaturewas refluxed
  2. concentrationconcentrated in vacuo
  3. custompartitioned between methylene chloride and water
  4. dry with materialThe organic phase was dried with magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-c081516339d44421813e9ed4b012269d
Quelldatensatz
uspto-grants-1987_04
Patentnummer
US04659706

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