Bromine → 3-acetyl-8-bromo-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine

HRID 542733Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 542733
[C:1]([N:4]1[CH2:10][CH2:9][C:8]2[CH:11]=[CH:12][C:13]([O:15][CH3:16])=[CH:14][C:7]=2[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[Br:17]Br>C(O)(=O)C>[C:1]([N:4]1[CH2:10][CH2:9][C:8]2[CH:11]=[C:12]([Br:17])[C:13]([O:15][CH3:16])=[CH:14][C:7]=2[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

Komponenten

4

Edukt 2

HCID 24408BromineHCID 138533493-acetyl-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine

Produkt 1

HCID 212428893-acetyl-8-bromo-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel2×

Versuchsvorschrift

A solution of 3-acetyl-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine (2.3 g, 0.01 m) in acetic acid (20 ml) is treated with a solution of bromine (1.8 g, 0.011 m) in acetic acid (10 ml). The mixture is warmed to 70° for 1.5 hours, concentrated in vacuo and partitioned between water and ethyl acetate. The ethyl acetate phase is washed, dried with sodium sulfate and concentrated in vacuo to give 3-acetyl-8-bromo-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine.

Aufarbeitung

  1. temperatureThe mixture is warmed to 70° for 1.5 hours
  2. concentrationconcentrated in vacuo
  3. custompartitioned between water and ethyl acetate
  4. washThe ethyl acetate phase is washed
  5. dry with materialdried with sodium sulfate
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-f27f01b034b6452cb205d456fa16d1f2
Quelldatensatz
uspto-grants-1987_04
Patentnummer
US04659706

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