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

HRID 621433Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 621433
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-036b219f2c4640baad59dbd5c93151c1
Quelldatensatz
uspto-grants-1989_04
Patentnummer
US04824839

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