Methanol → 3-Ethyl-7,8-dimethoxy-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine

HRID 972349Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 972349
[CH3:1][O:2][C:3]1[C:19]([O:20][CH3:21])=[CH:18][C:6]2[CH:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:8][NH:9][CH2:10][CH2:11][C:5]=2[CH:4]=1.[CH2:22](Br)[CH3:23].[OH-].[K+].CO>C(OCC)(=O)C>[CH3:1][O:2][C:3]1[C:19]([O:20][CH3:21])=[CH:18][C:6]2[CH:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:8][N:9]([CH2:22][CH3:23])[CH2:10][CH2:11][C:5]=2[CH:4]=1

Komponenten

6

Edukt 4

HCID 887MethanolHCID 6332Ethyl BromideHCID 14797Potassium HydroxideHCID 105409631H-3-Benzazepine, 2,3,4,5-tetrahydro-7,8-dimethoxy-1-phenyl-

Produkt 1

HCID 214066873-Ethyl-7,8-dimethoxy-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A sample of 7,8-dimethoxy-1-phenyl-2,3,4,5,-tetrahydro-1H-3-benzazepine weighing 4.32 g. (0.0154 mol), 2.18 g. (0.02 mol) of ethyl bromide and 1.12 g. (0.02 mol) of potassium hydroxide are dissolved in 120 ml. of dry methanol and the solution is refluxed overnight. Evaporation of the solution to dryness gives a mixture which is taken up in ethyl acetate and filtered to remove inorgaic salts. The filtrate is washed with water, dried and evaporated to give 7,8-dimethoxy-3-ethyl-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine as an oil.

Aufarbeitung

  1. customEvaporation of the solution to dryness
  2. customgives a mixture which
  3. filtrationfiltered
  4. customto remove inorgaic salts
  5. washThe filtrate is washed with water
  6. customdried
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-0eef670453494b7bb628cf3fcf679a1e
Quelldatensatz
uspto-grants-1977_10
Patentnummer
US04052506

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